U.S. patent application number 09/753569 was filed with the patent office on 2001-08-23 for silicone-treated powder, process of production thereof and composition containing the same.
This patent application is currently assigned to SHISEIDO COMPANY, LTD.. Invention is credited to Jouichi, Kyoko, Kanemaru, Tetsuya, Ohno, Kazuhisa.
Application Number | 20010016202 09/753569 |
Document ID | / |
Family ID | 18538190 |
Filed Date | 2001-08-23 |
United States Patent
Application |
20010016202 |
Kind Code |
A1 |
Kanemaru, Tetsuya ; et
al. |
August 23, 2001 |
Silicone-treated powder, process of production thereof and
composition containing the same
Abstract
A silicone-treated powder composed of a powder coated on the
surface thereof with a silicone compound, wherein an amount of
hydrogen generated by Si--H groups remained on the surface of the
silicone-treated powder is not more than 0.2 ml/g of treated powder
and a contact angle of water with the treated powder is at least
100.degree..
Inventors: |
Kanemaru, Tetsuya;
(Yokohama-shi, JP) ; Jouichi, Kyoko;
(Yokohama-shi, JP) ; Ohno, Kazuhisa;
(Yokohama-shi, JP) |
Correspondence
Address: |
Harold C. Wegner
FOLEY & LARDNER
Washington Harbour
3000 K Street, N. W., Suite 500
Washington
DC
20007-5109
US
|
Assignee: |
SHISEIDO COMPANY, LTD.
|
Family ID: |
18538190 |
Appl. No.: |
09/753569 |
Filed: |
January 4, 2001 |
Current U.S.
Class: |
424/401 ; 424/59;
424/64; 427/2.14 |
Current CPC
Class: |
A61Q 1/12 20130101; A61K
8/891 20130101; A61K 8/26 20130101; A61K 8/27 20130101; A61Q 1/02
20130101; C09C 1/3684 20130101; C09C 1/3081 20130101; C01P 2004/64
20130101; C09C 1/42 20130101; C09C 3/12 20130101; C01P 2004/62
20130101; A61K 8/11 20130101; C01P 2006/90 20130101; A61K 8/29
20130101; A61Q 1/06 20130101; A61K 8/19 20130101; A61K 8/585
20130101; B82Y 30/00 20130101; A61K 2800/412 20130101; C01P 2004/84
20130101; A61K 8/25 20130101; A61K 8/28 20130101; A61Q 17/04
20130101 |
Class at
Publication: |
424/401 ; 424/64;
424/59; 427/2.14 |
International
Class: |
A61K 007/025; A61K
007/42 |
Foreign Application Data
Date |
Code |
Application Number |
Jan 14, 2000 |
JP |
2000-10146 |
Claims
1. A silicone-treated powder comprising a powder coated on the
surface thereof with a silicone compound, wherein an amount of
hydrogen generated by Si--H groups remained on the surface of the
silicone-treated powder is not more than 0.2 ml/g of treated powder
and a contact angle of water with the treated powder is at least
100.degree..
2. A cosmetic composition comprising the silicone-treated powder
according to claim 1, as one ingredient of the formulating
material, and a carrier thereof.
3. A cosmetic composition as claimed in claim 2, wherein said
cosmetic composition is in the form of a solid foundation, emulsion
foundation, pressed powder, face powder, UV blocking stick,
lipstick, water-in-oil type emulsion sunscreen, or body powder.
4. A coating composition comprising a silicone-treated powder
according to claim 1, as one ingredient of the formulating
material, and a carrier thereof.
5. A resin molded article obtained by injection molding a synthetic
resin composition containing a silicone-treated powder according to
claim 1, as one ingredient of the formulating material and a
carrier thereof.
6. A process for producing a silicone-treated powder comprising the
steps of: coating a surface of a powder with (1) a silicone
compound having at least one Si--H group or (2) a mixture of the
silicone compound (1) and a silicone compound not having an Si--H
group; and then heating the silicone compound coated powder at a
temperature of 260 to 500.degree. C. for 0.1 to 24 hours.
7. A process for producing a silicone-treated powder as claimed in
claim 6, wherein an average particle size of the powder is not more
than 0.1 .mu.m and the silicone compound coated powder is heated in
the second step at a temperature of 260 to 350.degree. C. for 1 to
5 hours.
8. A process for producing a silicone-treated powder as claimed in
claim 6, wherein an average particle size of the powder is not less
than 0.1 .mu.m and the silicone compound coated powder is heated in
the second step at a temperature of 330 to 480.degree. C. for 1 to
5 hours.
9. A process for producing a silicone-treated powder as claimed in
claim 6, wherein said silicone compound having an Si--H group is a
silicone compound having the formula (1):
(R.sup.1HSiO).sub.a(R.sup.2R.sup.3SiO).s-
ub.b(R.sup.4R.sup.5R.sup.6SiO.sub.1/2).sub.c (1) wherein R.sup.1,
R.sup.2, and R.sup.3 independently represent a hydrogen atom or a
C.sub.1 to C.sub.10 hydrocarbon group, which may be substituted
with at least one halogen atom, provided that R.sup.1, R.sup.2 and
R.sup.3 are not simultaneously hydrogen atoms, R.sup.4, R.sup.5 and
R.sup.6 independently represent a hydrogen atom or a C.sub.1 to
C.sub.10 hydrocarbon group, which may be substituted with at least
one halogen atom, a is an integer of 1 or more, b is 0 or an
integer of 1 or more, c is 0 or 2, provided that
3.ltoreq.a+b+c.ltoreq.10000, and the compound has at least one
Si--H group.
10. A process for producing a silicone-treated powder as claimed in
claim 9, wherein said silicone compound having an Si--H group is
methylhydrogenpolysiloxane, a
methylhydrogenpolysiloxane-dimethylpolysilo- xane copolymer or
tetramethylcyclotetrasiloxane.
11. A process for producing a silicone-treated powder as claimed in
claim 6, wherein said heat treatment in the second step is carried
out in the air or under an atmosphere of one or more other gases
containing moisture of at least an extent of the moisture in the
air or under an atmosphere not containing moisture while adding
moisture.
12. A cosmetic composition comprising a silicone-treated powder
obtained by the process according to claim 6 as one ingredient of
the material and a carrier thereof.
13. A cosmetic composition as claimed in claim 12, wherein said
cosmetic composition is in the form of a solid foundation, emulsion
foundation, pressed powder, face powder, UV blocking stick,
lipstick, water-in-oil type emulsion sunscreen, and body
powder.
14. A coating composition comprising a silicone-treated powder
obtained by the production process according to in claim 6, as one
ingredient of the formulating material and a carrier thereof.
15. A resin molded article obtained by injection molding a
synthetic resin composition comprising a silicone-treated powder
obtained by the process according to claim 6, as one ingredient of
the formulating material and a carrier thereof.
Description
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to a process for producing a
silicone-treated powder, more specifically relates to a
silicone-treated powder obtained by coating a silicone compound
having an Si--H group on the surface thereof and polymerizing the
silicone on the surface thereof by heat treatment to obtain water
repellency and to eliminate almost all the residual Si--H groups on
the coating, to thereby be able to be formulated into various
cosmetics, and superior in stability in a product, and a production
process thereof.
[0003] 2. Description of the Related Art
[0004] There have been various methods for giving hydrophobicity to
a powder in the past. Using the hydrophobicity of silicone oil is
well known.
[0005] The silicone compounds usable for providing hydrophobicity
are those having an organohydrogenpolysiloxane chain in the
molecule and also sometimes having a diorganopolysiloxane chain in
the molecule or a mixture of organohydrogenpolysiloxane and
diorganopolysiloxane. When these compounds are coated on the
surface of a powder, the Si--H group bonded portion of the
organohydrogenpolysiloxane molecule reacts with the moisture etc.
in the air due to the surface activity of the powder, and the Si-OH
groups produced react with the Si--H groups of the other adjacent
molecules, or the Si-OH groups react among themselves to cause
cross-linking and polymerization and to form a silicone film.
[0006] However, with heat treatment in the air at about 200.degree.
C. after coating organohydrogenpolysiloxane on the surface of a
powder, the residual Si--H groups are not completely eliminated,
while the cross-linking reaction of the molecules themselves
proceeds to a certain extent. On the other hand, with heating at
500.degree. C. or more, the silicone starts to burn and is
converted to silica (see Japanese Unexamined Patent Publication
(Kokai) No. 11-199458, the treatment for coating silicon oxide by
heating at a temperature of 600 to 950.degree. C.
[0007] The residual Si--H groups react with the moisture in the air
or the moisture, alcohol, amines, etc. in makeup products over a
long period of time to cause the production of hydrogen and form
new siloxane bonds, and therefore, if the above treated powder is
used as it is for cosmetics, coating compositions, toners, inks,
containers, and ingredients of various other compositions, various
problems will sometimes be caused in the compositions.
[0008] For example, in the case of cosmetics, there is a risk of
generation of hydrogen in the production process, the containers
may swell with the elapse of time after filling the product into
containers, and the product may harden and crack. In the case of
coating compositions, the problem of deterioration of the container
sometimes occurs.
[0009] To reduce the above-mentioned residual Si--H groups, for
example, the method of Japanese Unexamined Patent Publication
(Kokai) No. 63-113081 (i.e., Japanese Patent No. 1635593) (i.e.,
the addition of a compound having unsaturated hydrocarbon group to
residual Si--H groups by hydrosilylation reaction), the method of
Japanese Unexamined Patent Publication (Kokai) No. 8-192101 (i.e.,
the substitution of residual Si--H groups by contact with water or
lower alcohol), the method of Japanese Examined Patent Publication
(Kokoku) No. 56-43264 (i.e., the mixture and pulverization of metal
hydroxide serving as a catalyst for cross-linking and
polymerization of organohydrogenpolysiloxane with a treated powder,
then using mechanochemical reaction), etc. have been attempted.
[0010] The above methods are effective in their own right, but the
processes are complicated, a long time is required, or relatively
active functional groups are adsorbed on the surface, and therefore
the powder is given an unpleasant smell etc.
SUMMARY OF THE INVENTION
[0011] In view of the above-mentioned situation, the object of the
present invention is to provide a silicone-treated powder free from
generation of hydrogen and having a good quality and also a process
for producing such a silicone-treated powder and a process of
production having a reduced manufacturing cost.
[0012] That is, according to the present invention, there is
provided a silicone-treated powder comprising a powder coated on
the surface thereof with a silicone compound wherein an amount of
hydrogen generated by Si--H groups remained on the surface of the
silicone-treated powder is not more than 0.2 ml/g of treated powder
and a contact angle of water with the treated powder is at least
100.degree..
[0013] In accordance with the present invention, there is also
provided a process for producing a silicone-treated powder
comprising the steps of:
[0014] coating a surface of a powder with
[0015] (1) a silicone compound having at least one Si--H group or
(2) a mixture of the silicone compound (1) and a silicone compound
not having an Si--H group and; then
[0016] heating the silicone compound coated powder at a temperature
of 260 to 480.degree. C. for 0.1 to 24 hours.
[0017] Here, when the average particle size of the powder is not
more than 0.1 .mu.m, the silicone compound coated powder is
preferably heated in the second step at 260 to 350.degree. C. for 1
to 5 hours, while when the average particle size of the powder is
not less than 0.1 .mu.m, the silicone compound coated powder is
preferably heated in the second step at 330 to 480.degree. C. for 1
to 5 hours.
[0018] In accordance with the present invention, there are further
provided a cosmetic composition comprising the above
silicone-treated powder, as one ingredient of the formulating
material and a carrier thereof, a coating composition comprising
the above silicone-treated powder as one ingredient of the
formulating material and a carrier thereof, and a resin molded
article obtained by injection molding a synthetic resin composition
containing the silicone-treated powder as one ingredient of the
formulating material. Here, the cosmetic composition preferably
includes a solid foundation, emulsion foundation, pressed powder,
face powder, UV blocking stick, lipstick, water-in-oil type
emulsion sunscreen, and body powder.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0019] The present invention will now be explained in more detail.
In this specification and in the claims the singular forms "a",
"an" and "the" include plural referents unless the context clearly
dictates otherwise.
[0020] The present inventors engaged in intensive research and, as
a result, found that by heating a powder coated with
organohydrogenpolysiloxane etc. at a temperature of 260 to
480.degree. C., it is possible to cross-link or substitute with
inert functional groups almost all of the residual Si--H groups
while maintaining the hydrophobicity, whereby the present invention
was completed.
[0021] The powder usable in the present invention is not
particularly limited, but includes, for example, an organic
pigment, inorganic pigment, metal oxide, metal hydroxide, mica,
pearl agent, metal, magnetic powder, silicate ore, resin powder,
powder having rubber elasticity, or a porous substance alone or in
any combination thereof.
[0022] Particularly preferable powders among these are any
inorganic powders having particle sizes of not more than 1 mm
(sometimes including particles larger than 1 mm). Specifically,
metal oxides, metal hydroxides, clay minerals, pearl agents,
metals, carbon, magnetic powder, silicate ores, porous materials,
etc. are exemplified.
[0023] These powders may be used alone or in any combination
thereof. Further, they may be in a coagulated mass or in the form
of a molded or shaped article. According to the present invention,
it is possible to modify (or treat) any inorganic powder including
even superfine powder having a particle size of not more than 0.02
.mu.m.
[0024] Here, specific examples of the inorganic pigments (including
metal oxides and metal hydroxides), include, for example, Prussian
Blue, Ultramarine, Mangan Violet, titanium (oxide) coated mica,
magnesium oxide, aluminum oxide, aluminum hydroxide, silica, iron
oxides (.alpha.-Fe.sub.2O.sub.3, .gamma.-Fe.sub.2O.sub.3,
Fe.sub.3O.sub.4, FeO, FeOOH, etc.), yellow iron oxide, black iron
oxide, iron hydroxides, titanium oxides, in particular titanium
dioxide having a particle size of 0.001 to 1 .mu.m, lower titanium
oxide, cerium oxide, zirconium oxide, chromium oxide, chromium
hydroxide, manganese oxide, cobalt oxide, nickel oxide, etc. and
composite oxides and composite hydroxides obtained by combinations
of two or more of the same, for example, silica-alumina, iron
titanate, cobalt titanate, lithium cobalt titanate, cobalt
aluminate, etc. In addition, the nonoxides include bismuth
oxychloride, boronitride, silicon nitride, titanium nitride, and
other nonoxide ceramic powders.
[0025] The silicone-treated powder of the present invention has
almost all of the residual Si--H groups cross-linked or substituted
with inert functional groups and has no active functional groups
adsorbed on the surface, and therefore is a silicone-treated powder
which is almost completely free of generation of hydrogen, exhibits
sufficient hydrophobicity, and is stable and good in quality.
[0026] The amount of hydrogen generated by the Si--H groups
remained on the surface of the silicone-treated powder of the
present invention is not more than 0.2 ml/g of treated powder, more
preferably not more than 0.1 ml/g of treated powder. If the amount
of the generated hydrogen is more than 0.2 ml/g of treated powder,
there is an accompanying risk at the time of production of a
cosmetic or the shelf life of the product is obstructed in some
cases. Further, the contact angle of water with the treated powder
is not less than 100.degree., more preferably 100 to 130.degree..
If the contact angle of water is less than 100.degree., the
functions and stability of the product are sometimes hindered.
[0027] The silicone-treated powder of the present invention may be
produced by the above production process a silicone-treated powder
according to the present invention. The silicone compound having an
Si--H group in the silicone compounds usable for the process of
production includes those having the following general formula
(1):
(R.sup.1HSiO).sub.a(R.sup.2R.sup.3SiO).sub.b(R.sup.4R.sup.5R.sup.6SiO.sub.-
1/2).sub.c (1)
[0028] wherein R.sup.1, R.sup.2 and R.sup.3 independently represent
a hydrogen atom or a C.sub.1 to C.sub.10 hydrocarbon group, which
may be substituted with at least one halogen atom, provided that
R.sup.1, R.sup.2 and R.sup.3 are not simultaneously hydrogen atoms,
R.sup.4, R.sup.5 and R.sup.6 independently represent a hydrogen
atom or a C.sub.1 to C.sub.10 hydrocarbon group, which may be
substituted with at least one halogen atom, a is an integer of 1 or
more, b is 0 or an integer of 1 or more, c is 0 or 2, provided that
3.ltoreq.a+b+c.ltoreq.10000, and the above-mentioned compound
includes at least one Si--H group is preferable.
Methylhydrogenpolysiloxane, a
methylhydrogenpolysiloxane-dimethylpolysilo- xane copolymer or
tetramethylcyclotetrasiloxane is more preferable.
[0029] The silicone compounds other than silicone compounds having
an Si--H group usable in the process of the present invention
include, for example, dimethylpolysiloxane,
octamethylcyclotetrasiloxane, etc.
[0030] The amount of the silicone compound based upon the weight of
the powder usable in the process of the present invention is 0.1 to
20.0% by weight, preferably 0.5 to 15.0% by weight. If the amount
is too large, the usability or applicability (e.g., smoothness
etc.) naturally owned by the powder is largely lost. Contrary to
this, if the amount is too small, the intended water repellency is
not likely to be obtained.
[0031] In the production process of a silicone-treated powder of
the present invention, in the first step (i.e., the silicone
treatment step,), the silicone compound is brought into contact
with the above-mentioned various powders in the form of a vapor
thereof, in the form of a solution dissolved in a suitable solvent,
or in the form of a liquid thereof.
[0032] When the silicone compound is brought into contact with the
powder in the form of, for example, a vapor, a cyclic
organosiloxane and powder are placed in separate containers in a
sealed space and the tops left open or a treatment agent is mixed
with a carrier gas and introduced into a chamber loaded with the
powder, and therefore, no special apparatus is required.
[0033] When the silicone compound is brought into direct contact
with the powder in the form of a liquid, a suitable mixer, for
example, a rotary ball mixer, a vibration type ball mixer, a
planetary type ball mixer, a sand mill, an attritor, a bag mill, a
pony mixer, a planetary mixer, automated mortar, a Henschel mixer,
etc. may be used.
[0034] When the silicone compound is brought into contact with the
powder in, for example, a solution, a solution containing 0.3 to
50% by weight of the compound in a solvent such as alcohol, water,
hexane, cyclohexane, and toluene is prepared, the powder is
dispersed therein, then the solution heated to evaporate the
solvent and the silicone compound is polymerized on the surface.
This may be done using a Henschel mixer, a kneader, a mill using
beads, etc.
[0035] In the production process of a silicone-treated powder of
the present invention, in the second step of heat treating the
powder with which the silicone compound is mixed, the heating
temperature and time of the powder is 260 to 480.degree. C. for 0.1
to 24 hours, preferably 1 to 4 hours. If the temperature less than
260.degree. C., the Si--H groups do not easily react, while if more
than 480.degree. C., the burning and decomposition of the
Si-CH.sub.3 groups are promoted, and the hydrophobicity declines or
disappears (hydrophilicity), that is, the silicone is converted to
silica. Further, the production process of the silicone-treated
powder of the present invention differs in preferable treatment
conditions in the second step due to the average particle size of
the material powder. That is, if the average particle size of the
material powder is not more than 0.1 .mu.m, in the second step, the
silicone compound coated powder is preferably heated at 260 to
350.degree. C., preferably 270 to 320.degree. C. for 1 to 5 hours,
preferably 2 to 3 hours. When the average particle size of the
material powder is more than 0.1 .mu.m, in the second step, the
silicone compound coated powder is preferably heated at 330 to
480.degree. C., preferably 390 to 400.degree. C. for 1 to 5 hours,
preferably 1 to 2 hours.
[0036] Further, as the heating atmosphere, it is possible to heat
the powder in the air, which is an atmosphere containing moisture,
or in another gas containing moisture of an extent of the moisture
in the air. In addition, it is possible to adjust the powder in an
atmosphere not containing moisture, then heat while adding moisture
during the treatment or heating. As the device used for heating, an
electric furnace, tunnel furnace, roller hearth kiln, rotary kiln,
etc. may be used.
[0037] According to the present invention, there are further
provided a cosmetic composition, coating composition, and resin
molded article (e.g., container etc. formed by injection molding).
In the production processes of these compositions, it is possible
to produce products by ordinary methods other than the use of the
silicone-treated powder according to the present invention, instead
of powder treated by a conventional method. The cosmetic
composition, coating composition, and resin molded article obtained
in the present invention enable a reduction of the manufacturing
costs of the products, an improvement in the quality of the
products, stability of the products, and a reduction in the load in
work.
EXAMPLES
[0038] The present invention will now be further illustrated by,
but is by no means limited to, the following Examples. The units of
formulating amounts are % by weight.
[0039] (1) In the case of formulating powder material having an
average particle size of not less than 0.1 .mu.m
Example 1-1
[0040] 500 g of sericite (average particle size: 4 .mu.m) and 15 g
of methylhydrogenpolysiloxane (product name: Silicone KF99, made by
Shin-Etsu Chemical) were dissolved in 50 ml of hexane. This
solution was placed in a Henschel mixer and stirred and mixed at
room temperature for a predetermined time, then was placed in a
dryer of 100.degree. C. to evaporate the solvent. The powder was
then placed in an electric furnace set to 400.degree. C. in advance
and heated for 3 hours to obtain a silicone-treated powder.
Example 1-2
[0041] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 1-1 to titanium
dioxide (average particle size: 0.5 .mu.m).
Example 1-3
[0042] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 1-1 to silica
(average particle size: 5 .mu.m).
Example 1-4
[0043] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 1-1 to talc
(average particle size: 15 .mu.m).
Example 1-5
[0044] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 1-1 to zinc
white (average particle size: 0.5 .mu.m).
Example 1-6
[0045] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 1-1 to titanated
mica (average particle size: 20 .mu.m).
Example 1-7
[0046] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 1-1 to bengara
(average particle size: 0.4 .mu.m).
Example 1-8
[0047] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 1-1 to mica
(average particle size: 20 .mu.m).
Example 1-9
[0048] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 1-1 to golden
mica (average particle size: 30 .mu.m).
Example 1-10
[0049] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 1-1 to barium
sulfate (average particle size: 10 .mu.m).
Example 1-11
[0050] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 1-1 to a
titanium oxide/iron oxide composite (average particle size: 8
.mu.m).
Example 1-12
[0051] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 1-1 to
bengara-coated titanated mica (average particle size: 30
.mu.m).
Example 1-13
[0052] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 1-1 to a
cross-linked polysiloxane elastomer (average particle size: 5
.mu.m).
Example 1-14
[0053] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 1-1 to a
silicone resin coated/cross-linked polysiloxane elastomer (average
particle size: 5 .mu.m).
Example 1-15
[0054] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 1-1 to
polymethylsilsesquioxane powder (average particle size: 5
.mu.m).
Example 1-16
[0055] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 1-1 to
boronitride (average particle size: 20 .mu.m).
Example 1-17
[0056] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 1-1 to cerium
oxide powder (average particle size: 0.6 .mu.m).
Example 1-18
[0057] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 1-1 to chromium
oxide (average particle size: 0.5 .mu.m).
Example 1-19
[0058] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 1-1 to alumina
(average particle size: 0.3 .mu.m).
Example 1-20
[0059] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 1-1 to bismuth
oxychloride (average particle size: 3.0 .mu.m).
Example 2-1
[0060] The method of Example 1-1 was used to coat 500 g of sericite
with silicone, then this was placed in an electric furnace set to a
dry nitrogen atmosphere and raised in temperature. After reaching
400.degree. C., 10 g of water was dropped from above at a rate of
1/6 g/min. After dropping was finished, the powder was further
heated for 1 hour to obtain a silicone-treated powder.
Example 2-2
[0061] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 2-1 to titanium
dioxide (average particle size: 0.5 .mu.m).
Example 2-3
[0062] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 2-1 to silica
(average particle size: 5 .mu.m).
Example 2-4
[0063] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 2-1 to talc
(average particle size: 15 .mu.m).
Example 2-5
[0064] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 2-1 to zinc
white (average particle size: 0.5 .mu.m).
Example 2-6
[0065] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 2-1 to titanated
mica (average particle size: 20 .mu.m).
Example 2-7
[0066] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 2-1 to bengara
(average particle size: 0.4 .mu.m).
Example 2-8
[0067] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 2-1 to mica
(average particle size: 20 .mu.m).
Example 2-9
[0068] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 2-1 to golden
mica (average particle size: 30 .mu.m).
Example 2-10
[0069] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 2-1 to barium
sulfate (average particle size: 10 .mu.m).
Example 2-11
[0070] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 2-1 to a
titanium oxide/iron oxide composite (average particle size: 8
.mu.m).
Example 2-12
[0071] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 2-1 to
bengara-coated mica titanium (average particle size: 30 .mu.m).
Example 2-13
[0072] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 2-1 to a
cross-linked polysiloxane elastomer (average particle size: 5
.mu.m).
Example 2-14
[0073] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 2-1 to a
silicone resin coated/cross-linked polysiloxane elastomer (average
particle size: 5 .mu.m).
Example 2-15
[0074] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 2-1 to
polymethylsilsesquioxane powder (average particle size: 5
.mu.m).
Example 2-16
[0075] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 2-1 to
boronitride (average particle size: 20 .mu.m).
Example 2-17
[0076] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 2-1 to cerium
oxide powder (average particle size: 0.6 .mu.m).
Example 2-18
[0077] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 2-1 to chromium
oxide (average particle size: 0.5 .mu.m).
Example 2-19
[0078] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 2-1 to alumina
(average particle size: 0.3 .mu.m).
Example 2-20
[0079] The same procedure was followed to obtain a silicone-treated
powder except for changing the sericite of Example 2-1 to bismuth
oxychloride (average particle size: 3.0 .mu.m).
[0080] (2) In the case of the formulating powder material having an
average particle size of not more than 0.1 .mu.m
Example 3-1
[0081] 500 g of alumina-coated finely divided particle titanium
dioxide (average particle size: 0.015 .mu.m) and 25 g of
methylhydrogenpolysiloxa- ne were dissolved in 50 ml of hexane.
This solution was placed in a Henschel mixer and stirred and mixed
at room temperature for a predetermined time, then was placed in a
dryer of 100.degree. C. to evaporate the solvent. Next, the powder
was placed in an oven set to 270.degree. C. in advance and heated
for 3 hours to obtain a silicone-treated powder.
Example 3-2
[0082] The same procedure was followed to obtain a silicone-treated
powder except for changing the powder of Example 3-1 to finely
divided particle zinc oxide (average particle size: 0.01
.mu.m).
Example 3-3
[0083] The same procedure was followed to obtain a silicone-treated
powder except for changing the powder of Example 3-1 to finely
divided particle cerium oxide (average particle size: 0.01
.mu.m).
Example 4-1
[0084] 500 g of finely divided particle titanium dioxide (average
particle size: 0.01 .mu.m) and 35 g of
tetramethylcyclotetrasiloxane were placed in a desiccator and
allowed to stand at 50.degree. C. for one day, the powder was then
heated by passing through a tunnel furnace set to 300.degree. C. in
advance (nitrogen atmosphere containing moisture) over 10 minutes
to obtain a silicone-treated powder.
Example 4-2
[0085] The same procedure was followed to obtain a silicone-treated
powder except for changing the finely divided particle titanium
dioxide of Example 4-1 to finely divided particle zinc oxide
(average particle size: 0.01 .mu.m).
Example 4-3
[0086] The same procedure was followed to obtain a silicone-treated
powder except for changing the finely divided particle titanium
dioxide of Example 4-1 to bengara (average particle size: 0.08
.mu.m).
Example 4-4
[0087] The same procedure was followed to obtain a silicone-treated
powder except for changing the finely divided particle titanium
dioxide of Example 4-1 to carbon black (average particle size: 0.05
.mu.m).
Example 4-5
[0088] The same procedure was followed to obtain a silicone-treated
powder except for changing the finely divided particle titanium
dioxide of Example 4-1 to titanium mica (average particle size:
0.08 .mu.m).
Example 4-6
[0089] The same procedure was followed to obtain a silicone-treated
powder except for changing the finely divided particle titanium
dioxide of Example 4-1 to a titanium dioxide/iron oxide sintered
composite (average particle size: 0.07 .mu.m).
Example 4-7
[0090] The same procedure was followed to obtain a silicone-treated
powder except for changing the finely divided particle titanium
dioxide of Example 4-1 to chromium oxide (average particle size:
0.09 .mu.m).
Example 4-8
[0091] The same procedure was followed to obtain a silicone-treated
powder except for changing the finely divided particle titanium
dioxide of Example 4-1 to Ultramarine (average particle size: 0.07
.mu.m).
Example 4-9
[0092] The same procedure was followed to obtain a silicone-treated
powder except for changing the finely divided particle titanium
dioxide of Example 4-1 to finely divided particle cerium dioxide
(average particle size: 0.01 .mu.m).
Example 5-1
[0093] 100 g of finely divided particle titanium dioxide (average
particle size: 0.015 .mu.m), 300 g of toluene, 7 g of a
methylhydrogenpolysiloxane- -dimethylsiloxane copolymer (product
name: Silicone KF9901), and 200 g of zirconia beads having a
diameter of 1 mm .phi. were placed in a 1 liter cup made of Teflon
and stirred and mixed for a predetermined time at a predetermined
temperature, then the toluene was distilled off in vacuo and the
remainder was heated under the temperature conditions of Example 3
(270.degree. C., 3 hours) to obtain a silicone-treated powder.
Example 5-2
[0094] The same procedure was followed to obtain a silicone-treated
powder except for changing the powder of Example 5-1 to finely
divided particle zinc oxide (average particle size: 0.01
.mu.m).
Example 5-3
[0095] The same procedure was followed to obtain a silicone-treated
powder except for changing the powder of Example 5-1 to finely
divided particle cerium oxide (average particle size: 0.01
.mu.m).
Comparative Examples 1-1 to 1-20
[0096] The same procedures were followed by the same powders and
the same methods as the corresponding Examples 1 to obtain
silicone-treated powders except for not performing the heating
step.
Comparative Examples 2-1 to 2-20
[0097] The same procedures were followed by the same powders and
the same methods as the corresponding Examples 1 to obtain
silicone-treated powders except for heating at 300.degree. C. for 3
hours.
Comparative Examples 3-1 to 3-20
[0098] The same procedures were followed by the same powders and
the same methods as the corresponding Examples 1 to obtain
silicone-treated powders except for heating at 550.degree. C. for 3
hours.
Comparative Examples 4-1 to 4-20
[0099] The same procedures were followed by the same powders and
the same methods as the corresponding Examples 2 to obtain
silicone-treated powders except for heating at 300.degree. C. for 3
hours.
Comparative Examples 5-1 to 5-20
[0100] The same procedures were followed by the same powders and
the same methods as the corresponding Examples 2 to obtain
silicone-treated powders except for heating at 550.degree. C. for 3
hours.
Comparative Examples 6-1 to 6-3
[0101] The same procedures were followed by the same powders and
the same methods as the corresponding Examples 3 to obtain
silicone-treated powders except for heating at 200.degree. C. for 3
hours.
Comparative Examples 7-1 to 7-3
[0102] The same procedures were followed by the same powders and
the same methods as the corresponding Examples 3 to obtain
silicone-treated powders except for heating at 550.degree. C. for 3
hours.
Comparative Examples 8-1 to 8-9
[0103] The same procedures were followed by the same powders and
the same methods as the corresponding Examples 4 to obtain
silicone-treated powders except for heating at 200.degree. C. for 3
hours.
Comparative Examples 9-1 to 9-9
[0104] The same procedures were followed by the same powders and
the same methods as the corresponding Examples 4 to obtain
silicone-treated powders except for heating at 550.degree. C. for 3
hours.
Comparative Examples 10-1 to 10-3
[0105] The same procedures were followed by the same powders and
the same methods as the corresponding Examples 5 to obtain
silicone-treated powders except for heating at 200.degree. C. for 3
hours.
Comparative Examples 11-1 to 11-3
[0106] The same procedures were followed by the same powders and
the same methods as the corresponding Examples 5 to obtain
silicone-treated powders except for heating at 550.degree. C. for 3
hours.
[0107] The amounts of generation of hydrogen gas of the
silicone-treated powders obtained in the Examples and the
Comparative Examples and their contact angles with water were
determined by the following methods:
[0108] The generation amount of hydrogen gas was determined by the
gas burette method. 2 g of silicone-treated powder and about 40 ml
of alcohol were placed in a three-necked flask. About 1 ml of 10%
NaOH aqueous solution was dropped in this by a closed system to
cause the production of hydrogen gas and the amount of production
of hydrogen (ml) per g was calculated.
[0109] The contact angle with water was determined by using an IR
tableting machine (diameter 13 mm) to prepare pellets of the
silicone-treated powders of the Examples and Comparative Examples
and then using an automatic contact angle meter (Model CA-Z) made
by Kyowa Kaimen Kagaku (average value for three measurements).
[0110] The results of the determination of the amounts of hydrogen
generation and the contact angles with water in the
silicone-treated powders obtained in the Examples and the
Comparative Examples are shown in Tables 1 to 7. The smaller the
amount of residual Si--H groups acting as the source of the
generation of hydrogen gas and the higher the contact angle, the
better.
1TABLE 1 Amount of Amount of genera- genera- tion of tion of
residual Contact residual Contact hydrogen angle hydrogen angle
Example (ml/g) (degree) Example (ml/g) (degree) Ex. 1-1 0.08 115
Ex. 2-1 0.03 120 Ex. 1-2 0.01 120 Ex. 2-2 0.0 110 Ex. 1-3 0.10 107
Ex. 2-3 0.03 115 Ex. 1-4 0.03 109 Ex. 2-4 0.01 112 Ex. 1-5 0.02 115
Ex. 2-5 0.01 120 Ex. 1-6 0.01 116 Ex. 2-6 0.0 123 Ex. 1-7 0.04 122
Ex. 2-7 0.02 107 Ex. 1-8 0.05 117 Ex. 2-8 0.03 124 Ex. 1-9 0.03 107
Ex. 2-9 0.01 120 Ex. 1-10 0.12 115 Ex. 2-10 0.0 105 Ex. 1-11 0.03
120 Ex. 2-11 0.0 121 Ex. 1-12 0.08 111 Ex. 2-12 0.10 120 Ex. 1-13
0.17 123 Ex. 2-13 0.08 104 Ex. 1-14 0.11 119 Ex. 2-14 0.05 125 Ex.
1-15 0.07 126 Ex. 2-15 0.03 117 Ex. 1-16 0.06 124 Ex. 2-16 0.02 129
Ex. 1-17 0.02 121 Ex. 2-17 0.0 128 Ex. 1-18 0.03 118 Ex. 2-18 0.0
117 Ex. 1-19 0.05 120 Ex. 2-19 0.01 126 Ex. 1-20 0.11 128 Ex. 2-20
0.04 129
[0111]
2TABLE 2 Amount of Amount of genera- genera- tion of tion of
residual Contact residual Contact Comp. hydrogen angle Comp.
hydrogen angle Example (ml/g) (degree) Example (ml/g) (degree)
Comp. 2.81 120 Comp. Ex. 1.88 117 Ex. 1-1 2-1 Comp. 1.35 122 Comp.
Ex. 0.98 125 Ex. 1-2 2-2 Comp. 2.45 109 Comp. Ex. 1.65 103 Ex. 1-3
2-3 Comp. 2.08 110 Comp. Ex. 1.22 114 Ex. 1-4 2-4 Comp. 1.55 115
Comp. Ex. 1.04 107 Ex. 1-5 2-5 Comp. 1.87 117 Comp. Ex. 1.13 124
Ex. 1-6 2-6 Comp. 2.14 120 Comp. Ex. 1.64 127 Ex. 1-7 2-7 Comp.
2.00 114 Comp. Ex. 1.33 110 Ex. 1-8 2-8 Comp. 2.33 105 Comp. Ex.
1.79 104 Ex. 1-9 2-9 Comp. 2.52 115 Comp. Ex. 1.50 113 Ex. 1-10
2-10 Comp. 1.10 120 Comp. Ex. 0.68 121 Ex. 1-11 2-11 Comp. 1.34 111
Comp. Ex. 0.90 120 Ex. 1-12 2-12 Comp. 3.02 123 Comp. Ex. 1.98 104
Ex. 1-13 2-13 Comp. 2.43 119 Comp. Ex. 1.07 125 Ex. 1-14 2-14 Comp.
2.59 126 Comp. Ex. 1.36 117 Ex. 1-15 2-15 Comp. 2.20 124 Comp. Ex.
1.25 129 Ex. 1-16 2-16 Comp. 1.55 121 Comp. Ex. 0.73 128 Ex. 1-17
2-17 Comp. 1.81 118 Comp. Ex. 0.88 117 Ex. 1-18 2-18 Comp. 1.12 120
Comp. Ex. 0.55 126 Ex. 1-19 2-19 Comp. 1.76 128 Comp. Ex. 0.90 129
Ex. 1-20 2-20
[0112]
3TABLE 3 Amount of Amount of genera- genera- tion of tion of
residual Contact residual Contact Comp. hydrogen angle Comp.
hydrogen angle Example (ml/g) (degree) Example (ml/g) (degree)
Comp. 0.0 0 Comp. Ex. 0.68 129 Ex. 3-1 4-1 Comp. 0.0 0 Comp. Ex.
0.55 116 Ex. 3-2 4-2 Comp. 0.0 0 Comp. Ex. 0.46 110 Ex. 3-3 4-3
Comp. 0.0 0 Comp. Ex. 0.70 103 Ex. 3-4 4-4 Comp. 0.0 0 Comp. Ex.
0.51 128 Ex. 3-5 4-5 Comp. 0.0 0 Comp. Ex. 0.39 110 Ex. 3-6 4-6
Comp. 0.0 0 Comp. Ex. 0.80 130 Ex. 3-7 4-7 Comp. 0.0 0 Comp. Ex.
0.95 103 Ex. 3-8 4-8 Comp. 0.0 0 Comp. Ex. 1.18 111 Ex. 3-9 4-9
Comp. 0.0 0 Comp. Ex. 0.77 120 Ex. 3-10 4-10 Comp. 0.0 0 Comp. Ex.
0.43 113 Ex. 3-11 4-11 Comp. 0.0 0 Comp. Ex. 0.69 108 Ex. 3-12 4-12
Comp. 0.0 0 Comp. Ex. 1.02 110 Ex. 3-13 4-13 Comp. 0.0 0 Comp. Ex.
0.54 131 Ex. 3-14 4-14 Comp. 0.0 0 Comp. Ex. 0.79 114 Ex. 3-15 4-15
Comp. 0.0 0 Comp. Ex. 1.20 121 Ex. 3-16 4-16 Comp. 0.0 0 Comp. Ex.
0.41 117 Ex. 3-17 4-17 Comp. 0.0 0 Comp. Ex. 0.67 124 Ex. 3-18 4-18
Comp. 0.0 0 Comp. Ex. 0.37 126 Ex. 3-19 4-19 Comp. 0.0 0 Comp. Ex.
0.84 116 Ex. 3-20 4-20
[0113]
4 TABLE 4 Amount of generation of residual Contact Comp. hydrogen
angle Example (ml/g) (degree) Comp. 0.0 0 Ex. 5-1 Comp. 0.0 0 Ex.
5-2 Comp. 0.0 0 Ex. 5-3 Comp. 0.0 0 Ex. 5-4 Comp. 0.0 0 Ex. 5-5
Comp. 0.0 0 Ex. 5-6 Comp. 0.0 0 Ex. 5-7 Comp. 0.0 0 Ex. 5-8 Comp.
0.0 0 Ex. 5-9 Comp. 0.0 0 Ex. 5-10 Comp. 0.0 0 Ex. 5-11 Comp. 0.0 0
Ex. 5-12 Comp. 0.0 0 Ex. 5-13 Comp. 0.0 0 Ex. 5-14 Comp. 0.0 0 Ex.
5-15 Comp. 0.0 0 Ex. 5-16 Comp. 0.0 0 Ex. 5-17 Comp. 0.0 0 Ex. 5-18
Comp. 0.0 0 Ex. 5-19 Comp. 0.0 0 Ex. 5-20
[0114]
5TABLE 5 Amount of Amount of genera- genera- tion of tion of
residual Contact residual Contact Comp. hydrogen angle Comp.
hydrogen angle Example (ml/g) (degree) Example (ml/g) (degree) Ex.
3-1 0.17 113 Comp. Ex. 0.38 119 6-1 Ex. 3-2 0.04 122 Comp. Ex. 0.26
128 6-2 Ex. 3-3 0.11 119 Comp. Ex. 0.36 115 6-3 Comp. Ex. 0.0 0 7-1
Comp. Ex. 0.0 0 7-2 Comp. Ex. 0.0 0 7-3
[0115]
6TABLE 6 Amount of Amount of genera- genera- tion of tion of
residual Contact residual Contact Comp. hydrogen angle Comp.
hydrogen angle Example (ml/g) (degree) Example (ml/g) (degree) Ex.
4-1 0.19 123 Comp. Ex. 0.50 126 8-1 Ex. 4-2 0.17 117 Comp. Ex. 0.89
120 8-2 Ex. 4-3 0.11 115 Comp. Ex. 0.73 113 8-3 Ex. 4-4 0.08 110
Comp. Ex. 0.44 116 8-4 Ex. 4-5 0.16 118 Comp. Ex. 0.53 126 8-5 Ex.
4-6 0.15 116 Comp. Ex. 0.67 110 8-6 Ex. 4-7 0.19 118 Comp. Ex. 0.90
127 8-7 Ex. 4-8 0.14 123 Comp. Ex. 0.70 121 8-8 Ex. 4-9 0.07 121
Comp. Ex. 0.56 117 8-9 Comp. Ex. 0.0 0 9-1 Comp. Ex. 0.0 0 9-2
Comp. Ex. 0.0 0 9-3 Comp. Ex. 0.0 0 9-4 Comp. Ex. 0.0 0 9-5 Comp.
Ex. 0.0 0 9-6 Comp. Ex. 0.0 0 9-7 Comp. Ex. 0.0 0 9-8 Comp. Ex. 0.0
0 9-9
[0116]
7TABLE 7 Amount of Amount of genera- genera- tion of tion of
residual Contact Compara- residual Contact hydrogen angle tive
hydrogen angle Example (ml/g) (degree) Example (ml/g) (degree) Ex.
5-1 0.10 115 Comp. Ex. 0.55 120 10-1 Ex. 5-2 0.0 120 Comp. Ex. 0.25
121 10-2 Ex. 5-3 0.02 115 Comp. Ex. 0.37 119 10-3 Comp. Ex. 0 0
11-1 Comp. Ex. 0 0 11-2 Comp. Ex. 0 0 11-3
Example 6
[0117] Foundation
8 Ingredient wt % (1) Treated powder of Example 1-1 35.0 (2)
Treated powder of Example 1-2 13.0 (3) Treated powder of Example
1-4 24.7 (4) Treated powder of Example 1-10 10.0 (5) Treated powder
of Example 1-7 1.0 (6) Treated powder of Example 1-8 2.5 (7)
Treated powder of Example 1-9 0.1 (8) Liquid paraffin 8.0 (9)
Sorbitan sesquioleate 3.5 (10) Glycerol 2.0 (11) Ethyl paraben
0.2
[0118] Process of Production
[0119] The ingredients (1) to (7) were mixed and pulverized by a
pulverizer. The resultant mixture was transferred to a high speed
blender, then the ingredient (10) was added and the result mixed.
Separately from this, the ingredients (8), (9), and (11) were
homogeneously mixed, then this was added to the above mixture and
further homogeneously mixed. The mixture was then treated by a
pulverizer and passed through a sieve to obtain a standard particle
size, then the resultant powder was compression molded to obtain a
solid foundation. The foundation thus obtained had a good hold.
Comparative Example 12
[0120] The same procedure was followed as in Example 6 to prepare a
foundation except for replacing ingredients (1) to (7) in the
foundation prepared in Example 6 with the ingredients of the
corresponding Comparative Example 1.
Comparative Example 13
[0121] The same procedure was followed as in Example 6 to prepare a
foundation except for replacing the ingredients (1) to (7) in the
foundation prepared in Example 6 with the ingredients of the
corresponding Comparative Example 2.
Comparative Example 14
[0122] The same procedure was followed as in Example 6 to prepare a
foundation except for replacing the ingredients (1) to (7) in the
foundation prepared in Example 6 with the ingredients of the
corresponding Comparative Example 3.
[0123] (1) Evaluation of Use
[0124] Samples held at 50.degree. C. for one month were evaluated
by the following criteria as for various aspects of usability
(removability, covering power, slip, use by a sponge wet with
water, cracking of the pack surface, hold, transparency, and water
resistance) by a panel of 20 women:
[0125] Evaluation Criteria
[0126] Very good: At least 17 women responded sample was good
[0127] Good: 12 to 16 women responded sample was good
[0128] Fair: 9 to 11 women responded sample was good
[0129] Poor: 5 to 8 women responded sample was good
[0130] Very poor: 4 or less women responded sample was good
[0131] (2) Evaluation of Shelf Life
[0132] Samples held at 50.degree. C. for one month were compared
for stability.
[0133] (3) Evaluation of SPF (UV Blocking Effect)
[0134] Samples held at 50.degree. C. for one month were measured
for in vitro SPF value by the Spectro Radiometer method.
[0135] The results of evaluation of the usability of the samples of
Example 6 and Comparative Examples 12 to 14 by the above criteria
after being held at 50.degree. C. for one month are shown in Table
8.
9 TABLE 8 Comp. Comp. Comp. Ex. 6 Ex. 12 Ex. 13 Ex. 14 Removability
Very good Fair Fair Fair Covering power Very good Fair Fair Fair
Slip Good Good Good Poor Use on sponge wet No problem No problem No
problem Caking with water Cracking of pack None Yes Yes None
surface
[0136] As will be understood from Table 8, Example 6 could be
applied with no problem even using water as a dual use type and was
superior in shelf life.
Example 7
[0137] Emulsion Foundation
10 Ingredient wt % (A) Ion exchanged water 43.5 Sodium chondroitin
sulfate 1.0 1,3-butylene glycol 3.0 Methyl paraben q.s. (B)
Dimethylpolysiloxane (20 cs) 16.0 Decamethylcyclopentasiloxane 5.0
Silicone resin 1.0 Cetylisooctanate 1.0 Polyoxyalkylene modified
organopolysiloxane 4.0 (modification rate 20%) Antioxidant q.s.
Fragrance q.s (C) Treated powder of Example 1-8 1.0 Treated powder
of Example 2-3 0.45 Treated powder of Example 2-4 0.2 Treated
powder of Example 1-2 11.7 Treated powder of Example 1-1 9.65
Treated powder of Example 2-7 2.0
[0138] Process of Production
[0139] The ingredients (B) were heated to melt, then the powders of
ingredient (C) were added and dispersed in them. Further, the
ingredients (A) melted and heated in advance were added to make an
emulsion, then the emulsion was cooled to room temperature to
obtain an emulsion foundation. The obtained emulsion foundation had
a good hold.
Comparative Example 15
[0140] The same procedure was followed as in Example 7 to obtain an
emulsion foundation except for replacing the ingredients (C) in the
emulsion foundation prepared in Example 7 with the ingredients of
the corresponding Comparative Example 1.
Comparative Example 16
[0141] The same procedure was followed as in Example 7 to obtain an
emulsion foundation except for replacing the ingredients (C) in the
emulsion foundation prepared in Example 7 with the ingredients of
the corresponding Comparative Example 2.
Comparative Example 17
[0142] The same procedure was followed as in Example 7 to obtain an
emulsion foundation except for replacing the ingredients (C) in the
emulsion foundation prepared in Example 7 with the ingredients of
the corresponding Comparative Example 3.
[0143] The results of evaluation of the usability of the samples
and shelf life of Example 7 and Comparative Examples 15 to 17 by
the above criteria after being held at 50.degree. C. for one month
are shown in Table 9.
11 TABLE 9 Comp. Ex. Comp. Ex. Comp. Ex. Ex. 7 15 16 17 Covering
power Good Fair Fair Fair Slip Good Fair Fair Poor Hold Very good
Good Good Very poor Shelf life No problem Container Container No
problem swelled swelled
[0144] As will be understood from Table 9, the emulsion foundation
prepared in Example 7 had a good hold and was superior in shelf
life as well.
Example 8
[0145] Emulsion Foundation (Solid Type)
12 Ingredient wt % (A) Ion exhanged water 43.5 Sodium glutamate 1.0
1,3-butylene glycol 5.0 Methyl paraben q.s. (B)
Dimethylpolysiloxane (20 cs) 4.0 Decamethylcyclopentasiloxane 16.0
Silicone resin 1.0 Cetyl isooctanate 1.0 Polyoxyalkylene modified
organopolysiloxane 4.0 (modification rate 20%) Antioxidant q.s.
Fragrance q.s. (C) Wax 5.0 (D) Treated powder of Example 1-2 8.0
Treated powder of Example 2-7 0.5 Treated powder of Example 3-1 6.0
Treated powder of Example 2-10 3.0 Silicone-treated black iron
oxide 0.1 Silicone-treated yellow iron oxide 1.4
[0146] Process of Production
[0147] The ingredients (B) were heated, then the ingredient (C) was
added and the mixture made to completely melt. Next, the powders of
ingredients (D) were added and dispersed while heating. Further,
the ingredients (A) melted and heated in advance were added to
create an emulsion. This was then cooled to room temperature to
obtain an emulsion foundation (solid type). The obtained emulsion
foundation had a good hold.
Comparative Example 18
[0148] The same procedure was followed as in Example 8 to obtain an
emulsion foundation except for replacing the ingredients (D) in the
emulsion foundation (solid type) prepared in Example 8 with the
ingredients of the corresponding Comparative Example 1 (for Example
3-1, Comparative Example 6-1).
Comparative Example 19
[0149] The same procedure was followed as in Example 8 to obtain an
emulsion foundation (solid type) except for replacing the
ingredients (D) in the emulsion foundation prepared in Example 8
with the ingredients of the corresponding Comparative Example 2
(for Example 3-1, Comparative Example 7-1)
[0150] The results of evaluation of the usability of the samples
and shelf life of Example 8 and Comparative Examples 18 to 19 by
the above criteria after being held at 50.degree. C. for one month
are shown in Table 10.
13 TABLE 10 Ex. 8 Comp. Ex. 18 Comp. Ex. 19 Covering power Good
Fair Fair Slip Good Fair Poor Hold Very good Good Very poor Shelf
life No problem Container No problem swelled
[0151] As will be understood from Table 10, the emulsion foundation
prepared in Example 8 had a good hold and was superior in shelf
life as well.
Example 9
[0152] Pressed Powder
14 Ingredient wt % (1) Treated powder of Example 1-5 30.0 (2)
Treated powder of Example 1-4 65.8 (3) Iron oxide pigment 0.1 (4)
Squalane 2.0 (5) 2-ethylhexyl palmitate 2.0 (6) Fragrance 0.1
[0153] Process of Production
[0154] The ingredients (1), (2), and (3) were mixed in a Henschel
mixer, then a heated mixture of the ingredients (4) and (5) was
sprayed on the mixture. These were mixed, then pulverized, then
molded into a dish to obtain a pressed powder. The obtained pressed
powder had a moisture retention effect, a good hold, and superior
shelf life as well.
Example 10
[0155] Body Powder
15 Ingredients wt % (A) Treated powder of Example 1-4 89.0 Treated
powder of Example 1-6 10.0 Coloring pigment q.s. (B) Treated powder
of Example 1-5 3.0 (C) Magnesium stearate 4.0 Liquid paraffin 1.0
Bactericide q.s. (D) Fragrance q.s.
[0156] Process of Production
[0157] The ingredients (A) were mixed by a blender, then the
ingredient (B) was added and mixed well. The ingredients (C) were
then added, the coloring adjusted, then the ingredient (D) was
sprayed on and then homogeneously mixed in. The mixture was
pulverized by a pulverizer, then passed through a sieve to obtain
the body powder. The body powder thus obtained had a high water
repellency.
Example 11
[0158] Lipstick
16 Ingredient wt % (1) Hydrocarbon wax 3.0 (2) Carnauba wax 1.0 (3)
Glyceryl isostearate 40.0 (4) Liquid paraffin 45.8 (5) Treated
powder of Example 1-3 4.0 (6) Mixed treated powders of Example 1-1
and Example 1-7 6.0 (7) Fragrance 0.2
[0159] Process of Production
[0160] The ingredients (1) to (4) were melted at 85.degree. C.,
then the ingredients (5) and (6) were added while stirring. Next,
while stirring, the ingredient (7) was added and the mixture packed
into a container. The obtained lipstick was superior in moisture
retention effect.
Example 12
[0161] Water-in-Oil Type Emulsion Sunscreen
17 Ingredient wt % (A) Decamethylcyclopentasiloxane Bal.
Dimethylpolysiloxane 5.0 Polyoxyethylene.cndot.methylpolysiloxane
3.0 copolymer Organic modified bentonite 1.0 (B) Treated powder of
Example 1-4 10.0 Treated powder of Example 2-1 7.0 Treated powder
of Example 2-2 10.0 Silicone elastic powder 3.0 Fragrance q.s.
Antioxidant q.s. (C) Ion exchanged water 35.0 Glycerin 5.0
Preservative q.s.
[0162] Process of Production
[0163] The (A) phase was heated to melt, then the (B) phase was
added and the mixture was homogeneously dispersed by a homomixer.
Then phase (C) was added gradually and stirred well, then
homogeneously emulsified by a homomixer. This was then stirred and
cooled to obtain a water-in-oil type emulsion sunscreen. The
obtained sunscreen had a high sunburn preventing effect.
Comparative Example 20
[0164] The same procedure was performed as in Example 12 to prepare
a water-in-oil type emulsion sunscreen except for replacing the
treated powder portion in the ingredients (B) in the water-in-oil
type emulsion sunscreen prepared in Example 12 with the ingredients
of the corresponding Comparative Example 1.
Comparative Example 21
[0165] The same procedure was performed as in Example 12 to prepare
a water-in-oil type emulsion sunscreen except for replacing the
treated powder portion in the ingredients (B) in the water-in-oil
type emulsion sunscreen prepared in Example 12 with the ingredients
of the corresponding Comparative Example 2.
Comparative Example 22
[0166] The same procedure was performed as in Example 12 to prepare
a water-in-oil type emulsion sunscreen except for replacing the
treated powder portion in the ingredients (B) in the water-in-oil
type emulsion sunscreen prepared in Example 12 with the ingredients
of the corresponding Comparative Example 3.
[0167] The results of evaluation of the usability, the SPF value,
and the shelf life of the samples of Example 12 and Comparative
Examples 20 to 22 by the above criteria after being held at
50.degree. C. for one month are shown in Table Table 11.
18 TABLE 11 Comp. Ex. Comp. Ex. Comp. Ex. Ex. 12 20 21 22 Slip Good
Fair Fair Poor Transparency Very good Good Good Fair Water Very
good Good Good Very poor resistance SPF 44 41 42 22 Shelf life No
problem Container Container No problem swelled swelled
[0168] Comparative Example 20 and Comparative Example 21 were good
in usability to a certain extent, but the containers swelled along
with time, Comparative Example 22 suffered from aggregation of the
powder due to the hydrophilicity and had a low SPF, but Example 12
was superior in all of the usability, shelf life, and SPF
value.
Example 13
[0169] Coating Composition
[0170] 20 g of the treated powder obtained in Example 1-2 and 18 g
of acrylic resin solution (Mn=48,200, Mn/Mw=2.56) were mixed
together with 70 g of glass beads by a paint shaker for 20 minutes
to obtain a coating composition. The coating composition obtained
was superior in stability over time.
Example 14
[0171] Container
[0172] The treated powder obtained in Example 2-1 was mixed in an
amount of 2% by weight in polyethylene. This was then injected
molded into a white polystyrene wide mouth vase.
Comparative Example 23
[0173] As a Comparative Example, the same procedure was used as in
Example 14 for injection molding except for using finely divided
particle titanium dioxide not treated with silicone.
[0174] 4 cm.times.4 cm sized pieces were cut from the wide mouth
vases of Example 14 and Comparative Example 23 and measured for UV
absorption spectra (diffusion reflection method), whereupon the
piece obtained from Example 14 was observed to have a higher UV
absorption effect.
[0175] As explained in detail above, the silicone-treated powder of
the present invention was stable in quality and free from any
unpleasant odor from the powder. Further, the silicone-treated
powder of the present invention can be used for cosmetic
compositions, paints, resin shaped articles, and a broad range of
other products.
[0176] Further, according to the production process of a
silicone-treated powder of the present invention, there are the
advantages that it is possible to produce a good quality
silicone-treated powder by a simple process and possible to provide
it at a low production cost.
* * * * *