OIL AGENT-CONTAINING SILICONE ELASTOMER PARTICLE AND USE THEREOF IN COSMETIC COMPOSITION, ETC.
20210113452 · 2021-04-22
Inventors
- Mari WAKITA (Ichihara-Shi, Chiba, JP)
- Hiroko TANIGUCHI (Ichihara-Shi, Chiba, JP)
- Yasue KANZAKI (Ichihara-shi, Chiba, JP)
- Seiji HORI (Ichihara-shi, Chiba, JP)
Cpc classification
A61Q17/04
HUMAN NECESSITIES
C08L83/14
CHEMISTRY; METALLURGY
C08L83/00
CHEMISTRY; METALLURGY
A61Q5/065
HUMAN NECESSITIES
C08L83/00
CHEMISTRY; METALLURGY
A61Q1/02
HUMAN NECESSITIES
A61K8/368
HUMAN NECESSITIES
C08K5/56
CHEMISTRY; METALLURGY
A61Q1/12
HUMAN NECESSITIES
C08L83/14
CHEMISTRY; METALLURGY
A61K8/8158
HUMAN NECESSITIES
A61K8/894
HUMAN NECESSITIES
A61K8/891
HUMAN NECESSITIES
A61K8/0241
HUMAN NECESSITIES
C08L91/00
CHEMISTRY; METALLURGY
A61K8/92
HUMAN NECESSITIES
A61K8/064
HUMAN NECESSITIES
C08K5/56
CHEMISTRY; METALLURGY
C08L91/00
CHEMISTRY; METALLURGY
A61K8/895
HUMAN NECESSITIES
A61K8/4946
HUMAN NECESSITIES
C08G77/20
CHEMISTRY; METALLURGY
A61K2800/412
HUMAN NECESSITIES
A61K8/735
HUMAN NECESSITIES
A61K8/8147
HUMAN NECESSITIES
C08G77/80
CHEMISTRY; METALLURGY
A61K8/8117
HUMAN NECESSITIES
International classification
A61K8/891
HUMAN NECESSITIES
A61K8/368
HUMAN NECESSITIES
A61K8/58
HUMAN NECESSITIES
A61K8/81
HUMAN NECESSITIES
A61K8/894
HUMAN NECESSITIES
A61K8/92
HUMAN NECESSITIES
A61Q1/02
HUMAN NECESSITIES
A61Q1/12
HUMAN NECESSITIES
A61Q17/04
HUMAN NECESSITIES
Abstract
Provided is an oil-including elastomer particle wherein at least two silicon atoms within the silicone elastomer particle are cross-linked through a silalkylene group with a carbon number of between 4 and 20, and having a structure that includes, in the silicone elastomer particle, an oil that is liquid at 40° C. In general, the mixture of oil and the cross-linking silicone composition can be cured in the form of emulsion particles. Also provided herein are uses of the oil-including elastomer particle and emulsion particles formed therefrom.
Claims
1. An oil-including silicone elastomer particle that includes, in the silicone elastomer particle, an oil that is a liquid at 40° C., and having a structure wherein at least two silicon atoms within the silicone elastomer particle are cross-linked through a silalkylene group with a carbon number between 4 and 20.
2. The oil-including silicone elastomer particle as set forth in claim 1, that is produced through a cross-linking reaction, in water, of a cross-linkable silicone emulsion particle produced through emulsification, in water, a mixture of a cross-linkable silicone composition that comprises at least an organopolysiloxane wherein there are at least two alkenyl groups, with carbon numbers between 4 and 20, within the molecule, and an oil that is liquid at 40° C., having a structure wherein at least two silicon atoms within the silicone elastomer particle are cross-linked through a silalkylene group with a carbon number between 4 and 20, to include, in the silicone elastomer particle, an oil that is liquid at 40° C. that is derived from the cross-linkable silicone emulsion particle.
3. The oil-including silicone elastomer particle as set forth in claim 1, wherein the oil that is liquid at 40° C. is a non-reactive oil that does not have a reactive functional group within the molecule.
4. The oil-including silicone elastomer particle as set forth in claim 1, wherein the oil that is liquid at 40° C. is selected from the group consisting of silicone oils, hydrocarbon oils, ester oils, and combinations thereof, and that have no reactive functional groups within the molecules.
5. The oil-including silicone elastomer particle as set forth in claim 1, wherein the inclusion proportion of oil that is a liquid at 40° C. is in a range of between 5 and 60 mass % with respect to the silicone elastomer particle as a whole.
6. The oil-including silicone elastomer particle as set forth in claim 1, wherein the average particle diameter measured through a laser diffraction/scattering method is between 0.5 and 20 μm.
7. The oil-including silicone elastomer particle as set forth in claim 1, wherein for the silicone elastomer particle in a state that does not include oil that is liquid at 40° C., the JIS-A hardness, measured through curing in the form of a sheet, in a state that does not include oil that is liquid at 40° C., the cross-linkable silicone composition that is used to form the silicone elastomer particle, is in a range between 10 and 80.
8. The oil-including silicone elastomer particle as set forth in claim 1, wherein the silalkylene groups included in the silicone elastomer particles are substantially only silalkylene groups with carbon numbers of between 4 and 8, where the inclusion proportion of silalkylene groups with carbon numbers of 3 and below is less than 5 mass % with respect to the silicone elastomer particle.
9. The oil-including silicone elastomer particle as set forth in claim 1, wherein the inclusion proportion of silicon atom-bound hydrogen is no greater than 300 ppm, per unit mass.
10. The oil-including silicone elastomer particle as set forth in claim 1, wherein the cross-linkable silicone composition used in the oil-including silicone elastomer particle is a cross linkable composition that comprises: (a) an organopolysiloxane having at least two alkenyl groups, with a carbon number between 4 and 20, per molecule; (b) an organohydrodiene polysiloxane having at least two silicon atom-bound hydrogen atoms per molecule; and arbitrarily (c) a hydrosilylation reaction catalyst; wherein the mole ratio of the alkenyl group inclusion proportion (Alk) of component (a) and the silicon atom-bound hydrogen atom inclusion proportion (H) of component (b) is in a range (H/Alk) of from 0.7 through 1.2.
11. A cosmetic raw material that includes the oil-including silicone elastomer particle as set forth in claim 1.
12. A cosmetic composition that includes the oil-including silicone elastomer particle as set forth in claim 1.
13. An organic resin additive that includes the oil-including silicone elastomer particle as set forth in claim 1.
14. An organic resin that includes the oil-including silicone elastomer particle as set forth in claim 1.
15. A method for manufacturing the oil-including silicone elastomer particle as set forth in claim 1, the method including steps (I) and (II): (I) forming a cross-linkable silicone emulsion particle through emulsifying, in water, a mixture that comprises: a cross-linkable silicone composition (A) that comprises: (a) an organopolysiloxane having at least two alkenyl groups, with a carbon number between 4 and 20, per molecule; (b) an organohydrodiene polysiloxane having at least two silicon atom-bound hydrogen atoms per molecule; and arbitrarily (c) a hydrosilylation reaction catalyst; wherein the mole ratio of the alkenyl group inclusion proportion (Alk) of component (a) and the silicon atom-bound hydrogen atom inclusion proportion (H) of component (b) is in a range (H/Alk) of from 0.7 through 1.2; and an oil (B) that is liquid at 40° C.; and (II) producing the oil-including silicone elastomer particle through curing, in the presence of the (c) hydrosilylation reaction catalyst, the cross-linkable silicone emulsion particle that was produced in step (I).
Description
EMBODIMENTS
[0157] The oil-including silicone elastomer particles, the manufacturing method thereof, and the cosmetics including the same, according to the present invention, will be explained in greater detail through the embodiments and the reference examples. However, the present invention is not limited to only these embodiments. Viscosities in the embodiments are values at 25° C. Moreover, the characteristics of the individual silicone particles are measured as below. Note that in the embodiments, unless otherwise noted “silicone particle” is a general term for a particle comprising a silicone cured material (a cured silicone particle), and does not include emulsions.
[JIS a Hardness of the Silicone Particles]
[0158] (1) An isopropyl alcohol solution of chloroplatinic acid and a curable silicone composition that is the raw material for the silicone particles, in a state that does not include oil, was heated for one hour at 150° C. in an oven, to cure into a sheet. The hardnesses thereof were measured by a JIS A hardness meter specified in JIS K 6253, and defined as the hardnesses of the oil-including silicone particles in a state wherein oil is not included.
[0159] (2) An isopropyl alcohol solution of chloroplatinic acid and a mixture of the oil and the curable silicone composition that is the raw material for the oil-including silicone particles was heated for one hour at 150° C. in an oven, to cure into a sheet. The hardnesses thereof were measured by a JIS A hardness meter specified in JIS K 6253, and defined as the hardnesses of the oil-including silicone particles.
[Amount of Residual SiH in the Silicone Particles]
[0160] An ethanol solution of potassium hydroxide with a density of 40%, in respect to a unit mass, was added to the cured silicone particles and allowed to rest for one hour, and hydrogen gas produced up until the reaction end point was reached was trapped, and through headspace gas chromatography, the amount of trapped hydrogen produced was measured, to measure the per-unit mass amount of remaining silicon atom-bound hydrogen atoms.
[Average Primary Particle Diameters of the Emulsion Particles]
[0161] In regard to the emulsions prior to addition of the platinum catalyst, the cross-linkable silicone emulsion particles were measured through a laser diffraction-type grain size distribution measuring instrument (LS-230, manufactured by Beckman Coulter), and the median diameter (the “50% particle size,” which is the particle size corresponding to 50% in the cumulative distribution) was defined as the average particle size and listed in the table as “Emulsion Particle Size μm.”
[AVERAGE PARTICLE DIAMETERS OF THE SILICONE PARTICLES (POWDER)]
[0162] With ethanol as the dispersing agent, the particle sizes of the cured silicone particles were measured using a laser diffraction-type grain-size distribution measuring instrument (LA-750, by Horiba, Ltd.), to list in the table, as “Cured Particle Diameter μm,” the values for the median diameter of the cured silicone particles in the ethanol (D90, in micrometer, which is the particle size corresponding to 50% in the cumulative distribution), and the arithmetic deviation (SD, in μm.sup.2), which indicates the variation in the particle size distribution). For the measurement samples, cured silicone particles (1 g) and ethanol (100 mL) were dispersed in a 300 mL cup using a stirring blade and ultrasonic vibration equipment.
[Method for Measuring the Quantity of Oil Absorbed by the Powder]
[0163] 1 g of cured silicone particles was placed in a 100 mL beaker, and oil (squalane or decamethyl cyclopentasiloxane (D5)) was dripped in, one drop at a time, while stirring the silicone particles slowly with a glass rod, and the volume of oil drips required to form a uniform paste of cured silicone particles and oil was calculated. The proportion of the volume of the oil dripped, in respect to the cured silicone particles, was defined as the quantity of oil absorbed (g).
[Method for Measuring the Amount of Absorption of Artificial Skin Oil]
[0164] The amount of absorption of the artificial skin oil (oil mixture), described below, was carried out using the same method as the method for measuring the amount of absorption of oil of the powder, described above.
[0165] Triglyceride oleate/oleic acid/squalane were mixed so as to have a mass ratio of 6/2/2 (hereinafter termed simply “artificial skin oil”).
[Method for Measuring the Bulk Density of the Silicone Particles]
[0166] 100 mL of cured silicone particles was placed in a 100 mL cup, cured silicone particles were scraped off the top of the cup, and the weight of the silicone particles, less the weight of the cup, was measured. The weight (g) of the cured silicone particles produced was divided by the volume (mL), to calculate the bulk density of the cured silicone particles.
[0167] The average formulas for components of (A) and component (B) used in the reference examples are listed below.
[0168] In the formulas below, “Vi” indicates a vinyl group that is expressed as CH.sub.2═CH—, “Me” indicates a methyl group that is expressed by CH.sub.3—, and “He” indicates a hexenyl group that is expressed by CH.sub.2═CH—CH.sub.4H.sub.8—.
Me.sub.2HeSiO—(Me.sub.2SiO).sub.57—(MeHeSiO).sub.3—SiHeMe.sub.2 [Chemical Formula 1-1]
[0169] Alkenyl group inclusion proportion: 2.7 wt %. Viscosity: 100 mPa.Math.s.
Me.sub.2HeSiO—(Me.sub.2SiO).sub.137—(MeHeSiO).sub.1.5—SiHeMe.sub.2 [Chemical Formula 1-2]
[0170] Alkenyl group inclusion proportion: 0.97 wt %. Viscosity: 420 mPa.Math.s.
Me.sub.2ViSiO—(Me.sub.2SiO).sub.165—SiViMe.sub.2 [Chemical Formula 1-3]
[0171] Alkenyl group inclusion proportion: 0.47 wt %. Viscosity: 360 mPa.Math.s.
(Me.sub.3SiO.sub.1/2).sub.2(Me.sub.2SiO.sub.2/2).sub.7(HMeSiO.sub.2/2).sub.11(MeSiO.sub.3/2).sub.1 [Chemical Formula 2-1]
[0172] Silicon atom-bonded hydrogen atom inclusion proportion: 0.825 wt %. Viscosity: 15 mPa.Math.s.
HMe.sub.2SiO—(Me.sub.2SiO).sub.60—Me.sub.2SiH [Chemical Formula 2-2]
[0173] Silicon atom-bonded hydrogen atom inclusion proportion: 0.043 wt %. Viscosity: 64 mPa.Math.s.
[0174] The types of oils used in the oil-including silicone elastomer particles in the embodiments and the reference examples, and the viscosities thereof at 25° C., were as follows. Note that these oils were liquid, with good fluidity, at 40° C.
[0175] Oil 1: Both-end trimethylsiloxylated dimethylpolysiloxane [0176] (Viscosity 100 mPa.Math.s at 25° C.)
[0177] Oil 2: Decamethyl cyclopentasiloxane [0178] (Viscosity 3.8 mPa.Math.s at 25° C.)
[0179] Oil 3: Side chain polyether-modified polysiloxane [0180] (Viscosity 130 mPa.Math.s at 25° C.)
[0181] Oil 4: Trimethyl pentaphenyl trisiloxane [0182] (Viscosity 175 mPa.Math.s at 25° C.)
[0183] Oil 5: Higher alkyl-modified polysiloxane with C16-alkyl groups on the side chain [0184] (Viscosity 45 mPa.Math.s at 25° C.)
Embodiment 1: C6 Silicone Elastomer Particles Including 33% Oil 1
[0185] A polyorganosiloxane, expressed by the average formula of [Chemical Formula 1-2], and a polyorganosiloxane expressed by the average formula of [Chemical Formula 2-1] were mixed uniformly at room temperature with a mass ratio of 89:11, after which the oil 1, described above, was added in an amount so as to be 33% of the composition as a whole (that is, so that the oil inclusion proportion in the oil-including silicone elastomer particles after curing would be 33%), and mixed, to produce a cross-linkable composition. Following this, the composition was dispersed into an aqueous solution at 25° C. made from 3.0 parts by weight of polyoxyethylene alkyl (C12-14) ether and 20 parts by weight purified water, and following uniform emulsification using a colloid mill, this was diluted through adding 350 parts by weight purified water, to prepare an emulsion that includes a cross-linkable silicone emulsion particle comprising the cross-linkable silicone composition described above and oil 1. Next an isopropyl alcohol solution of chloroplatinic acid (in an amount such that the platinum metal in the composition will be 10 ppm, in terms of mass) was formed into an aqueous solution, with polyoxyethylene alkyl (C12 through 14) ether and purified water, and added to the emulsion, and after stirring, the emulsion was allowed to rest for three hours at 50° C., to prepare a uniform aqueous suspension of the oil-including silicone elastomer particles. Following this, the aqueous solution was dried using a small spray dryer (manufactured by Ashizawa-Niro), to produce the oil-including silicone elastomer particles. The physical properties, such as the JIS-A hardness, of the oil-including silicone elastomer particles produced are shown in Table 1.
Embodiment 2: C6 Silicone Elastomer Particles Including 40% Oil 1
[0186] Aside from adding the oil 1 in an amount so as to be 40% of the composition as a whole (that is, in an amount so that the oil inclusion proportion in the oil-including silicone elastomer particles after curing would be 40%), oil-including silicone elastomer particles were produced in the same manner as in the first embodiment. The physical properties, such as the JIS-A hardness, of the oil-including silicone elastomer particles produced are shown in Table 1.
Embodiment 3: C6 Silicone Elastomer Particles Including 30% Oil 1
[0187] A polyorganosiloxane, expressed by the average formula of [Chemical Formula 1-1], and a polyorganosiloxane expressed by the average formula of [Chemical Formula 2-1] were mixed uniformly at room temperature with a mass ratio of 89:11, after which the oil 1, described above, was added in an amount so as to be 33% of the composition as a whole (that is, so that the oil inclusion proportion in the oil-including silicone elastomer particles after curing would be 33%), and mixed, to produce a cross-linkable composition. Following this, the composition was dispersed into an aqueous solution at 25° C. made from 3.0 parts by weight of polyoxyethylene alkyl (C12-14) ether and 20 parts by weight purified water, and following uniform emulsification using a colloid mill, this was diluted through adding 350 parts by weight purified water, to prepare an emulsion that includes a cross-linkable silicone emulsion particle comprising the cross-linkable silicone composition described above and oil 1. Next an isopropyl alcohol solution of chloroplatinic acid (in an amount such that the platinum metal in the composition will be 10 ppm, in terms of mass) was formed into an aqueous solution, with polyoxyethylene alkyl (C12 through 14) ether and purified water, and added to the emulsion, and after stirring, the emulsion was allowed to rest for three hours at 50° C., to prepare a uniform aqueous suspension of the oil-including silicone elastomer particles. Following this, the aqueous solution was dried using a small spray dryer (manufactured by Ashizawa-Niro), to produce the oil-including silicone elastomer particles. The physical properties, such as the JIS-A hardness, of the oil-including silicone elastomer particles produced are shown in Table 1.
Embodiment 4: C6 Silicone Elastomer Particles Including 33% Oil 2
[0188] An aqueous suspension of oil-including silicone elastomer particles was produced in the same manner as in Embodiment 1, except for producing a uniform aqueous suspension of oil-including silicone elastomer particles according to each of the embodiments produced through this manufacturing process through adding the same amount of an oil 2, instead of the oil 1, and not removing the water content. The physical properties, such as the JIS-A hardness, of the oil-including silicone elastomer particles produced are shown in Table 1. Note that for this embodiment, the oil absorption was not measured directly.
Embodiment 5: C6 Silicone Elastomer Particles Including 33% Oil 3
[0189] An oil-including silicone elastomer particle was produced in the same manner as with Embodiment 1, except for replacing the oil 1 with the same amount of an oil 3. The physical properties, such as the JIS-A hardness, of the oil-including silicone elastomer particles produced are shown in Table 1. Note that because the oil 3 was a polyether modified silicone, the oil-including silicone elastomer particles produced were extremely superior in dispersibility in water.
Embodiment 6: C6 Silicone Elastomer Particles Including 20% Oil 4
[0190] Aside from adding an oil 4, instead of the oil 1, in an amount so as to be 20% of the composition as a whole (that is, in an amount so that the oil inclusion proportion in the oil-including silicone elastomer particles after curing would be 20%), oil-including silicone elastomer particles were produced in the same manner as in the first embodiment. The physical properties, such as the JIS-A hardness, of the oil-including silicone elastomer particles produced are shown in Table 1.
Embodiment 7: C6 Silicone Elastomer Particles Including 10% Oil 5
[0191] Aside from adding an oil 5, instead of the oil 1, in an amount so as to be 10% of the composition as a whole (that is, in an amount so that the oil inclusion proportion in the oil-including silicone elastomer particles after curing would be 10%), oil-including silicone elastomer particles were produced in the same manner as in the first embodiment. The physical properties, such as the JIS-A hardness, of the oil-including silicone elastomer particles produced are shown in Table 1.
Reference Example 1: Vinyl (C2) Cross-Linked Silicone Particles Including 33% Oil 1
[0192] An oil-including silicone elastomer particle was produced in the same manner as with Embodiment 1 except for the use of a vinyl (C2) group-including polyorganosiloxane, expressed by the average formula [Chemical Formula 1-3] instead of the polyorganosiloxane expressed by the average formula of [Chemical Formula 1-1], and a polyorganosiloxane expressed by the average formula of [Chemical Formula 2-2], instead of the polyorganosiloxane expressed by the average formula of [Chemical Formula 2-1], at a mass ratio of 95:5. The physical properties, such as the JIS-A hardness, of the oil-including silicone elastomer particles produced are shown in Table 1.
Reference Example 2: C6 Cross-Linked Silicone Elastomer Particles, not Including Oil
[0193] Oil-including silicone elastomer particles were produced in the same manner as in Embodiment 1, except that oil 1 was not used. The physical properties, such as the JIS-A hardness, of the oil-including silicone elastomer particles produced are shown in Table 1.
Reference Example 3: C6 Cross-Linked Silicone Elastomer Particles, Not Including Oil
[0194] Oil-including silicone elastomer particles were produced in the same manner as in Embodiment 1, except that oil 3 was not used. The physical properties, such as the JIS-A hardness, of the oil-including silicone elastomer particles produced are shown in Table 1.
TABLE-US-00001 TABLE 1 Population Powder Powder Skin Amount JIS JIS Emulsion Cured Oil Oil Oil of Cross- Hardness Hardness Particle Particle Absorption Absorption Absorption remaining Bulk linked Oil (No (With Size Size Amount Amount Amount SiH Density Alkylene Oil Amount % Oil) Oil) μm μm *1 g *2 g *3 g ppm g/ml Embod- C6 1 33 20 9 7.9 73.7 0.32 0.61 0.20 0.08 0.34 iment 1 Embod- 1 40 20 7 7.9 61.3 0.32 0.33 0.13 0.20 0.36 iment 2 Embod- 1 33 30 15 7.5 39.8 0.20 0.28 0.12 0.90 0.41 iment 3 Embod- 2 33 20 10 5.0 3.5 Aqueous suspension, so not measured. iment 4 Embod- 3 33 20 6 6.4 27.5 0.04 0.09 0.05 — 0.53 iment 5 Embod- 4 20 20 11 8.7 39.2 0.25 2.40 0.13 — 0.61 iment 6 Embod- 5 10 20 1 8.6 99.9 0.31 0.39 0.24 — 0.49 iment 7 Reference C2 1 33 30 15 7.4 38.1 0.86 0.89 0.56 77.7 0.22 Example 1 Reference C6 1 0 20 — 8.3 92.0 0.38 3.44 0.30 0.40 0.30 Example 2 Reference 1 0 30 — 7.3 35.1 0.34 2.72 0.40 1.40 0.36 Example 3 *1: Amount of squalane absorbed *2: Amount of decamethyl cyclopentane siloxane (D5) absorbed *3: Amount of absorption of artificial skin oil (mixture of triglyceride oleate/oleic acid/squalane with a mass ratio of 6/2/2)
[0195] As depicted in Table 1, the oil-including silicone elastomer particles according to Embodiments 1 through 3 were confirmed to have low oil absorption, whether for squalane, which is an organic oil, or D5, which is a silicone-based oil. In particular, when compared with Reference Example 1, which is an existing oil-including silicone particle (vinyl cross-linked), the oil-including silicone elastomer particles according to the present embodiment had low oil absorption for both squalane and D5. Moreover, when compared to Reference Example 2 and Reference Example 3, which are silicone particles cross-linked with hexenyl groups (C6), the same as in the embodiments, there was remarkably low oil absorption, particularly for D5, which is a silicone-based oil. Moreover, as seen in the evaluation result using artificial skin oil, the oil-including silicone elastomer particles according to the embodiments, when compared to the reference examples, have low oil absorption. Because of this, there is little effect, when mixing the preparations, on cosmetic amounts, or the like, from organic oils, silicone-based oils, and skin oils, and it can be anticipated that, on the skin, there will be little absorption of skin oil.
<Evaluation of Agglomeration>
[0196] Through the same method as for the average particle diameters for the silicone particles (powder), described above, the particle diameters, both initially and after storage at 50° C. (for one month) of the silicone particles produced were measured, and the rate of change thereof was recorded (in the table below).
TABLE-US-00002 TABLE 2 Change in Cured Particle Diameters in Embodiments 1 and 3 and in Reference Example 1 Cured Particle Rate of Diameter after Change Initial Cured Storage for One in the Particle Month at 50° C. Particle Diameter (Median (Median Diameter) Diameter Diameter) (μm) (μm) (%) Embodiment 1 73.7 57.4 −22% Embodiment 3 39.8 49.7 +25% Reference 38.1 87.3 +129% Example 1
[0197] Although they are oil-including silicone particles using the same oil, in Embodiment 1 and Embodiment 3 there was no large change in the particle diameters (median diameters) after high temperature storage, while, in contrast, in Reference Example 1, which is a cross-linking structure derived from vinyl groups, the particle diameter (median diameter) after high temperature storage was more than twice as large, confirming that there was severe advancement of agglomeration with the passage of time. Given this, the oil-including silicone particles in the present embodiment not only have low oil absorption, but are also able to suppress agglomeration, and thus can be anticipated to have superior storage stability and ease of handling.
[0198] In the preparation disclosed in Patent Document 3 (Japanese Unexamined Patent Application Publication H02-243612), described below, oil-including silicone elastomer particles obtained through Embodiment 3, above (inclusion proportion of oil 1: 33%) and silicone particles of Reference Example 1 were used to prepare oily foundations for evaluation. Moreover, as a reference test, a powder/oil blend was prepared through impregnation of the silicone elastomer particles of Reference Example 3 with 33% oil 1, and then subjected to the same evaluation.
Embodiment 8, Reference Example 4, and Reference Examples: Oily Foundations
(Method of Preparation)
[0199] After mixing Phase B, described in Table 3, below, until uniform using a blender mixer, Phase A, described in Table 3, below, was heated to 70° C. and added, and stirred until uniform. The sample produced was transferred to a container and cooled until room temperature.
(Method of Evaluation)
<Appearance of Sample>
[0200] ∘: Of the 10 panel members, at least seven answered “has a uniform surface.”
[0201] Δ: Of the 10 panel members, four to six answered “has a uniform surface.”
[0202] x: Of the 10 panel members, no more than three answered “has a uniform surface.”
<Color Nonuniformity>
[0203] ∘: Of the 10 panel members, at least seven answered “color is uniform.”
[0204] Δ: Of the 10 panel members, four to six answered “color is uniform.”
[0205] x: Of the 10 panel members, no more than three answered “color is uniform.”
<Spreading on Skin>
[0206] ∘: Of the 10 panel members, at least seven answered “spreads well on skin.”
[0207] Δ: Of the 10 panel members, four to six answered “spreads well on skin.”
[0208] x: Of the 10 panel members, no more than three answered “spreads well on skin.”
TABLE-US-00003 TABLE 3 Composition of Oily Foundation Ingredient Brand Name/Supplier Embodiment 8 Reference Examples Reference Example 4 Phase A Microcrystalline Refined 4 4 4 wax Microcrystalline Wax/Nikko Rica Ozokerite Ceresin 4 4 4 #810/Nikko Rica Lanolin Alcohol .fwdarw. Behenyl 2 2 2 Replacement Alcohol/Nihon Emulsion Liquid Paraffin Hicall 3 3 3 R-230/Kaneda Sorbitan EMALEX 1 1 1 Sesquioleate SPO-150/ Nihon Emulsion Decamethyl Toray • Dow 35 35 35 Cyclopentasiloxane Corning/SH245 Isopropyl Myristate EXCEPAL 2 2 2 IPM/Kao Phase B Pigment-grade SI-Titanium 15.7 15.7 15.7 Titanium Oxide CR-50/Miyoshi Kasei Yellow Iron Oxide SA 1.8 1.8 1.8 Yellow/Miyoshi Kasei Red Iron Oxide SA-Bengalese 0.4 0.4 0.4 cloisonne/ Miyoshi Kasei Black Iron Oxide SA 0.9 0.9 0.9 Black/Miyoshi Kasei Kaolin White Clay/ 20 20 20 Alban Muller International Talc JR-46 R/Asada 5 5 5 Seifun Oil-including 6 Silicone Elastomer Particle of Embodiment 3 (Including Oil 1 at 33%) Powder/Oil Blend 6 *1 (Including Oil 1 at 33%) Silicone Particle of 6 Reference Example 1 (Including Oil 1 at 33%) Appearance of Sample ◯ ◯ x Color Nonuniformity ◯ Δ x Spreading on Skin ◯ Δ x *1: In respect to the silicone particles of reference example 3 powder/oil blend wherein oil 1 is added at an amount to be 33 mass % overall
[0209] As shown in Table 3, for the powder part, when compared in an identical oily foundation, the oil-including silicone elastomer particles of the embodiment were superior in all evaluations in respect to Reference Example 1, which is an existing oil-including silicone particle (vinyl cross-linked). Moreover, for reference, in a powder/oil blend wherein the same amount of oil was added to a silicone elastomer particle, cross-linked by the same hexenyl groups as in the embodiments, the evaluation in terms of appearance was the same, but the color nonuniformity, the quality of the cosmetic spread on the skin, and the feel in use were not on par with those of the embodiments. Given the evaluations set forth above, the oil-including silicone elastomer particle according to the present invention can be used as a cosmetic raw material that provides cosmetics with superior appearance and feel in use, and these characteristics can be anticipated.
[0210] Examples of preparations of cosmetics according to the present invention, in which the oil-including silicone particles that are one form of the present invention can be mixed, are presented below. However, the present invention is not limited thereto. Note that, unless otherwise specified, in the preparations below the “oil-including silicone elastomer particles according to the present embodiment” may refer, without any particular limitation, to any of the oil-including silicone elastomers of Embodiments 1 through 3 and 5 through 7, described above, or to mixtures of two or more thereof. Note that the aqueous suspension of Embodiment 4 may be used as-is as an aqueous preparation.
Preparation Example 1: W/O Cream Foundation
(Ingredients)
[0211]
TABLE-US-00004 Phase A Cetyl diglycerol tris (trimethylsiloxy) 5.0 parts by weight silyl ethyl dimethicone (Note 1) 2) Dimethicone (Note 2) 4.2 parts by weight 3) Ethylhexyl methoxysilicic acid (Note 3) 3.3 parts by weight 4) Caprylyl methicone (Note 4) 3.3 parts by weight 5) lsododecane and (dimethicone/bis- 1.5 parts by weight isobutyl PPG-20) cross-polymer (Note 5) 6) Oil-including silicone elastomer particles 2.0 parts by weight according to the present embodiment Phase B 7) Titanium oxide, talc, methicone (Note 6) 4.71 parts by weight 8) Mica, aluminum hydroxide (Note 7) 2.46 parts by weight 9) Yellow iron oxide (Note 8) 0.66 parts by weight 10) Red iron oxide (Note 9) 0.16 parts by weight 11) Black iron oxide (Note 10) 0.006 parts by weight 12) Cetyl diglycerol tris (trimethylsiloxy) 0.5 parts by weight silyl ethyl dimethicone (Note 11) 13) Caprylyl methicone (Note 12) 3.7 parts by weight Phase C 14) Purified water 61.5 parts by weight 15) BG 8.0 parts by weight 16) Sodium chloride 1.0 parts by weight Note 1: ES-5600 Silicone Glycero Emulsifier, manufactured by Toray Dow Corning Co. Note 2: PMX-200 SILICONE FLUID 2CS, manufactured by Toray Dow Corning Co. Note 3: Neo Heliopan AV, manufactured by Symrise Note 4: FZ-3196, manufactured by Toray Dow Corning Co. Note 5: EL-8050 ID Silicone Organic Elastomer Blend, manufactured by Toray Dow Corning Co. Note 6: SA Titan CR-50, manufactured by Miyoshi Kasei Note 7: SA Exel Mica JP-2, manufactured by Miyoshi Kasei Note 8: SA Yellow UXLO, manufactured by Miyoshi Kasei Note 9: SA Red, manufactured by Miyoshi Kasei Note 10: SA Black, manufactured by Miyoshi Kasei Note 11: ES-5600 Silicone Glycero Emulsifier, manufactured by Toray Dow Corning Co. Note 12: FZ-3196, manufactured by Toray Dow Corning Co.
[0212] The W/0 cream foundation of Preparation 1 was prepared using the procedure described below:
[0213] 1. Ingredients 1 through 6 were mixed until uniform.
[0214] 2. Ingredients 7 through 13 were mixed using a three-roller milling machine.
[0215] 3. Ingredients 14 through 16 were mixed.
[0216] 4. 1 and 2, above, were mixed.
[0217] 5. While agitating 4, above, vigorously, 3 was added to perform emulsification.
Preparation 2: 0/W Foundation
[0218] (Ingredients)
TABLE-US-00005 Phase A 1) Oil-including silicone elastomer particles 18 parts by weight according to the present embodiment 2) Talc (Note 1) 18 parts by weight Phase B 3) Purified water 20 parts by weight 4) Glycerin 10 parts by weight Phase C 5) Sodium polyacrylate, methicone (Note 2) 1 part by weight 6) DMDM hydantoin, propynyl A suitable amount butylcarbamate iodide (Note 3) 7) Ethylhexyl salicylic acid (Note 4) 3 parts by weight 8) Ethylhexyl methoxysilicic acid (Note 5) 3 parts by weight Phase D 9) Purified water 21 parts by weight Phase E 10) Caprylyl methicone (Note 6) 2 parts by weight 11) Black iron oxide, methicone (Note 7) 0.05 parts by weight 12) Red iron oxide, methicone (Note 8) 0.1 parts by weight 13) Yellow iron oxide, methicone (Note 9) 0.25 parts by weight 14) Titanium oxide, talc, dimethicone 3.6 parts by weight (Note 10) Note 1: Si talc, manufactured by Miyoshi Kasei Note 2: RM 2051 Rheology Modifier, manufactured by Toray Dow Corning Co. Note 3: Glydant Plus, manufactured by Lonza Note 4: Neo Heliopan OS, manufactured by Symrise Note 5: Escalol 557, manufactured by ISP Note 6: FZ-3196, manufactured by Toray Dow Corning Co. Note 7: SA-black BL-100, manufactured by Miyoshi Kasei Note 8: SA-Bengalese cloisonne, manufactured by Miyoshi Kasei Note 9: SI-YELLOW-LLXL0, manufactured by Miyoshi Kasei Note 10: SI-titanium CR-50, manufactured by Miyoshi Kasei
[0219] The O/W cream foundation of Preparation 2 was prepared using the procedure described below:
[0220] 1. Ingredients 1 and 2 were mixed.
[0221] 2. Ingredients 3 and 4 were mixed.
[0222] 3. 1 and 2, above, were mixed.
[0223] 4. Ingredients 5 through 8 were mixed.
[0224] 5. Ingredient 9 was added to 4, above, and mixed.
[0225] 6. Ingredients 10 through 14 were mixed until uniform.
[0226] 7. All ingredients were mixed.
Preparation 3: W/0 BB Cream
[0227] (Ingredients)
TABLE-US-00006 Phase A 1) Lauryl PEG-10 Tris (Trimethylsiloxy) 3 parts by weight silyl ethyl dimethicone (Note 1) 2) Caprylyl methicone (Note 2) 14 parts by weight 3) Ethylhexyl methoxysilicic acid (Note 3) 7.5 parts by weight 4) Hexyl diethylaminohydroxybenzoyl 1.5 parts by weight benzoate (Note 4) 5) Ethylhexyl salicylic acid 2.5 parts by weight 6) Trimethylsiloxysilicate, polypropylene 2 parts by weight silsesquioxane (Note 5) 7) Oil-including silicone elastomer 4 parts by weight particles according to the present embodiment 8) Phenyl trimethicone (Note 6) 4 parts by weight Phase B 9) Glycerin 8 parts by weight 10) Sodium chloride 0.7 parts by weight 11) Purified water 40.8 parts by weight Phase C 12) Titanium oxide 5.6 parts by weight 13) Yellow iron oxide (Note 7) 0.25 parts by weight 14) Red iron oxide (Note 8) 0.1 parts by weight 15) Black iron oxide (Note 9) 0.05 parts by weight 16) Phenyl trimethicone (Note 10) 5.2 parts by weight 17) Zinc oxide (Note 11) 0.8 parts by weight 18) Lauryl PEG-10 Tris (Trimethylsiloxy) 1 part by weight silyl ethyl dimethicone Note 1: ES-5300 Formulation Aid, manufactured by Toray Dow Corning Co. Note 2: FZ-3196, manufactured by Toray Dow Corning Co. Note 3: UVINUL MC80N, manufactured by BASF Note 4: A Plus Glanular, manufactured by BASF Note 5: MQ-1640 Flake Resin, manufactured by Toray Dow Corning Co. Note 6: SH556, manufactured by Toray Dow Corning Co. Note 7: SA-IOY-8, manufactured by Miyoshi Kasei Note 8: SA-IOR-8, manufactured by Miyoshi Kasei Note 9: SA-IOB-8, manufactured by Miyoshi Kasei Note 10: SH556, manufactured by Toray Dow Corning Co. Note 11: FINEX-30S-LPT, manufactured by Sakai Chemical Industry Co. Note 12: ES-5300 Formulation Aid, manufactured by Toray Dow Corning Co.
[0228] The BB cream of Preparation 3 was prepared using the procedure described below:
[0229] 1. Ingredients 1 through 8 were mixed.
[0230] 2. Ingredients 9 through 11 were mixed.
[0231] 3. Ingredients 12 through 18 were mixed.
[0232] 4. 1 and 3, above, were mixed.
[0233] 5. While agitating 1, above, vigorously, 2 was added slowly to perform emulsification.
Preparation 4: Nonaqueous Foundation
[0234] (Ingredients)
TABLE-US-00007 Phase A 1) Titanium oxide, dimethicone (Note 1) 49.23 parts by weight 2) Yellow iron oxide, methicone (Note 2) 9.86 parts by weight 3) Red iron oxide, methicone (Note 3) 1.97 parts by weight 4) Black iron oxide, methicone (Note 4) 0.55 parts by weight 5) Cetyl diglycerol tris (trimethylsiloxy) 1.58 parts by weight silyl ethyl dimethicone (Note 5) 6) Caprylyl methicone (Note 6) 15.8 parts by weight Phase B 7) Oil-including silicone elastomer particles 2 parts by weight according to the present embodiment 8) Cyclopentasiloxane (Note 7) 13 parts by weight 9) lsododecane, (acrylate/polytrimethylsiloxyl 5 parts by weight methacrylate) copolymer (Note 8) 10) Disteardimonium hectorite (Note 9) 1 part by weight Note 1: SI-titanium CR-50, manufactured by Miyoshi Kasei Note 2: SI-YELLOW-LLXLO, manufactured by Miyoshi Kasei Note 3: SA-Bengalese cloisonne, manufactured by Miyoshi Kasei Note 4: SA-black BL-100, manufactured by Miyoshi Kasei Note 5: ES-5600 Silicone Glycero Emulsifier, manufactured by Toray Dow Corning Co. Note 6: FZ-3196, manufactured by Toray Dow Corning Co. Note 7: SH245, manufactured by Toray Dow Corning Co. Note 8: FA 4002 ID Silicone Acrylate, manufactured by Toray Dow Corning Co. Note 9: Bentone (R) 38 V CG, manufactured by Elementis
[0235] The nonaqueous foundation of Preparation 4 was prepared using the procedure described below:
[0236] 1. Ingredients 1 through 6 were mixed.
[0237] 2. Ingredients 7 through 10 were mixed.
[0238] 3. 1 and 2, above, were mixed.
Preparation 5: Compact Foundation
[0239] (Ingredients)
TABLE-US-00008 1) Talc (Note 1) 20 parts by weight 2) Mica (Note 2) 34.6 parts by weight 3) Titanium oxide (Note 3) 10 parts by weight 4) Red iron oxide (Note 4) 1 part by weight 5) Yellow iron oxide (Note 5) 4 parts by weight 6) Black iron oxide (Note 6) 0.4 parts by weight 7) Mica (Note 7) 15 parts by weight 8) Polystyrene (Note 8) 5 parts by weight 9) Squalane 3 parts by weight 10) Octyldodecyl myristic acid (Note 9) 1.2 parts by weight 11) Vaseline 2.5 parts by weight 12) Dimethicone (Note 10) 3.3 parts by weight 13) Oil-including silicone elastomer particles 5 parts by weight according to the present embodiment Note 1: Si Talc, manufactured by Miyoshi Kasei Note 2: SI-SERICITE FSE, manufactured by Miyoshi Kasei Note 3: SI-Titan CR-50, manufactured by Miyoshi Kasei Note 4: SA Red, manufactured by Miyoshi Kasei Note 5: SA Yellow UXLO, manufactured by Miyoshi Kasei Note 6: SA Black, manufactured by Miyoshi Kasei Note 7: SA Excel Mica JP-2, manufactured by Miyoshi Kasei Note 8: Fine pearl 3000SPQ, manufactured by Sumitomo Chemical Note 9: EXCEPARL OD-M, manufactured by Kao Note 10: SH200-5000cs, manufactured by Toray Dow Corning Co.
[0240] The compact foundation of Preparation 5 was prepared using the procedure described below:
[0241] 1. All of the above were mixed.
Preparation 6: W/O Skin Cream
[0242] (Ingredients)
TABLE-US-00009 Phase A 1) Lauryl PEG/PPG-18/18 dimethicone 2 parts by weight (Note 1) 2) Bis (hydroxyethoxypropyl) dimethicone 2 parts by weight (Note 2) 3) Isopropyl palmitic acid (Note 3) 1 part by weight 4) Cyclopentasiloxane (Note 4) 6.5 parts by weight 5) Mineral oil (Note 5) 10 parts by weight 6) Vaseline 1.5 parts by weight 7) Oil-including silicone elastomer particles 5 parts by weight according to the present embodiment Phase B 8) Glycerin 5 parts by weight 9) Sodium chloride 1 part by weight 10) Purified water 66 parts by weight Note 1: 5200 Formulation Aid, manufactured by Toray Dow Corning Co. Note 2: 5562 Carbinol Fluid, manufactured by Toray Dow Corning Co. Note 3: EXCEPAL IPM, manufactured by Kao Note 4: SH245, manufactured by Toray Dow Corning Co. Note 5: Hicall K-230, manufactured by Kaneda
[0243] The W/O skin cream of Preparation 6 was prepared using the procedure described below:
[0244] 1. Ingredients 1 through 7 were mixed.
[0245] 2. Ingredients 8 through 10 were mixed.
[0246] 3. While agitating 1, above, vigorously, 2 was added slowly to perform emulsification.
Preparation 7: Sunblock Nonaqueous Lotion
[0247] (Ingredients)
TABLE-US-00010 1) Zinc oxide (Note 1) 6 parts by weight 2) Lauryl PEG-10 Tris (Trimethylsiloxy) 0.5 parts by weight silyl ethyl dimethicone (Note 2) 3) Hexadecane 3.5 parts by weight 4) Ethylhexyl methoxysilicic acid 7.5 parts by weight (Note 3) 5) Dimethicone, dimethicone cross- 24 parts by weight polymer (Note 4) 6) Cyclopentasiloxane (Note 5) 60.5 parts by weight 7) Oil-including silicone elastomer 2 parts by weight particles according to the present embodiment Note 1: FINEX-30S-LPT, manufactured by Sakai Chemical Industry Co. Note 2: ES-5300 Formulation Aid, manufactured by Toray Dow Corning Co. Note 3: UVINUL MC80N, manufactured by BASF Note 4: 9041 Silicone Elastomer Blend, manufactured by Toray Dow Corning Co. Note 5: SH245, manufactured by Toray Dow Corning Co.
[0248] The sunblock nonaqueous lotion of Preparation 7 was prepared using the procedure described below:
[0249] 1. Ingredients 1 through 3 were mixed (using a bead mill, or the like).
[0250] 2. Ingredients 4 through 7 were added to the ingredients above and agitated until uniform.
Preparation 8: 0/W Wrinkle Cream
[0251] (Ingredients)
TABLE-US-00011 Phase A 1) Cyclopentasiloxane (Note 1) 11 parts by weight 2) Oil-including silicone elastomer 10 parts by weight particles according to the present embodiment 3) Lauryl PEG/PPG-18/18 0.5 parts by weight dimethicone (Note 2) 4) PEG-12 dimethicone (Note 3) 4 parts by weight Phase B 5) Purified water 72.5 parts by weight Phase C 6) Polyacrylamide, water, 2 parts by weight (C13, 14) isoparaffin, LAURETH-7 (Note 4) Note 1: SH245, manufactured by Toray Dow Corning Co. Note 2: 5200 Formulation Aid, manufactured by Toray Dow Corning Co. Note 3: OFX-5329, manufactured by Toray Dow Corning Co. Note 4: Simulgel 305, manufactured by SEPPIC S.A.
[0252] The O/W wrinkle cream of Preparation 8 was prepared using the procedure described below:
[0253] 1. Ingredients 1 through 4 were mixed until uniform.
[0254] 2. Ingredients 4 and 5 were mixed until uniform.
[0255] 3. 1, above, was added to 2, and mixed until uniform.
Preparation 9: Toilet Water
[0256] (Ingredients)
TABLE-US-00012 Phase A 1. Silicone emulsifier premix *1 7.0 parts by weight 2. Trilaurez-4 phosphoric acid *2 0.05 parts by weight 3. Ethanol 2.0 parts by weight Phase B 4. Water Remainder 5. Butylene glycol (BG) 3.0 parts by weight 6. Glycerin 6.0 parts by weight 7. Dipropylene glycol (DPG) 2.0 parts by weight 8. Disodium hydrogen phosphate 0.01 parts by weight 9. Sodium dihydrogen phosphate 0.01 parts by weight 10. Preservatives Suitable amount 11. Oil-including silicone elastomer particles 5.0 parts by weight according to the fifth embodiment *1: FB-2540 Emulsifier Blend, manufactured by Toray Dow Corning Co. *2: Hostaphat KL340D, manufactured by Clariant
[0257] (Method of Preparation)
[0258] 1. Phase A is mixed.
[0259] 2. Phase B is mixed.
[0260] 3. While agitating phase B, phase A is added slowly.
Preparation 10: W/O Sunblock
[0261] (Ingredients)
TABLE-US-00013 Phase A 1. Silicone emulsifier *1 1.5 parts by weight 2. Ethylhexyl methoxysilicic acid *2 7.5 parts by weight 3. Hexyl diethylaminohydroxybenzoyl 2.0 parts by weight benzoate *3 4. Caprylyl methicone *4 2.0 parts by weight 5. lsotridecyl isonononate *5 3.0 parts by weight 6. lsohexadecane 8.0 parts by weight 7. Silicone film forming agent *6 1.0 parts by weight 8. Disteardimonium hectorite *7 1.0 parts by weight Phase B 9. Fine titanium oxide *8 6.0 parts by weight 10. Silicone dispersing agent *9 1.5 parts by weight 11. lsohexadecane 7.5 parts by weight Phase C 12. Butylene glycol (BG) 7.0 parts by weight 13. Sodium citrate 0.2 parts by weight 14. Sodium chloride 0.5 parts by weight 15. Water Remainder Phase D 16. Oil-including silicone elastomer 3.0 parts by weight particles according to the present embodiment *1: ES-5300 Formulation Aid, manufactured by Toray Dow Corning Co. *3: UVINUL MC80N, manufactured by BASF *3: UVINUL A Plus, manufactured by BASF *4: FZ-3196, manufactured by Toray Dow Corning Co. *5: Emalex INTD-139, manufactured by Nihon Emulsion Co. *6: FA-4002ID Silicone Acrylate, manufactured by Toray Dow Corning Co. *7: Benton 38V, manufactured by Elementis *8: MTY-02, manufactured by TAYCA *9: ES-5600 Silicone Glycero Emulsifier, manufactured by Toray Dow Corning Co.
[0262] (Method of Preparation)
[0263] 1. Phase A is mixed.
[0264] 2. Phase B is mixed.
[0265] 3. Phase C is mixed.
[0266] 4. Phase A and phase B are mixed.
[0267] 5. While agitating phases AB, phase C is added slowly.
[0268] 6. Phase D is added, and agitated until uniform.
Preparation 11: 0/W Sunblock
[0269] (Ingredients)
TABLE-US-00014 Phase A 1. Polysorbate 80 *1 1.0 parts by weight 2. Mineral oil *2 10 parts by weight 2. Triethyl hexanoate 5.0 parts by weight 3. Hexyl diethylaminohydroxybenzoyl 2.5 parts by weight benzoate *3 4. Ethylhexyl methoxysilicic acid *4 7.5 parts by weight 5. Caprylyl methicone *5 10 parts by weight 6. Oil-including silicone elastomer 5.0 parts by weight particles according to the present embodiment 7. Titanium oxide dispersion *6 10 parts by weight Phase B 8. Carbomer 2% aqueous solution *7 15 parts by weight 9. Water Remainder 10. Sodium hydroxide 1% aqueous Suitable amount solution 11. Butylene glycol (BG) 5.0 parts by weight 12. Glycerin 2.0 parts by weight *1: Leodore TW-0120V, manufactured by Kao *2: Hicall K-230, manufactured by Kaneda *3: UVINUL A Plus, manufactured by BASF *4: UVINUL MC80N, manufactured by BASF *5: FZ-3196, manufactured by Toray Dow Corning Co. *6: MTY-02 40 wt %, cyclopentasiloxane 50 wt %, ES-5600 Silicone Glycerol Emulsifier 10 wt %, manufactured by TAYCA *7: Carbopol 980, manufactured by Lubrizol
[0270] (Method of Preparation)
[0271] Phase A is mixed.
[0272] Phase B is mixed.
[0273] While agitating phase B, phase A is added slowly.
Preparation 12: Toilet Water Sheet
[0274] (Ingredients)
TABLE-US-00015 Phase A 1. (Acrylate/alkyl acrylate (C10-30)) 0.1 part by weight cross-polymer *1 2. Water Remainder 3. Sodium hydroxide Suitable amount Phase B 4. Glycerin 4.0 parts by weight 5. Oil-including silicone elastomer 2.0 parts by weight particles according to the present embodiment 6. Aloe vera water 0.6 parts by weight 7. Panthenol 0.3 parts by weight 8. Water 5.0 parts by weight Phase C 9. Alkyl benzoate (012-15) 2.7 parts by weight 10. Polysorbate 20 *2 0.5 parts by weight 11. Cross-linked silicone gel *3 3.5 parts by weight 12. Cyclopentasiloxane *4 5.8 parts by weight 13. Preservatives Suitable amount 14. Fragrance Suitable amount *1: Carbopol ETD2020, manufactured by Lubrizol *2: Tween20, manufactured by Croda *3: 9041 Silicone Elastomer Blend, manufactured by Toray Dow Corning Co. *4: SH245 Oil, manufactured by Toray Dow Corning Co.
[0275] (Method of Preparation)
[0276] Phase A is mixed.
[0277] While agitating phase A, phase B is added.
[0278] While agitating phase AB vigorously, phase C is added.
[0279] The emulsion described above is impregnated into a nonwoven fabric.
Preparation 13: Cosmetic Foundation
[0280] (Ingredients)
TABLE-US-00016 Phase A 1. Titanium oxide *1 3.0 parts by weight 2. Mica 10 parts by weight 3. Styrene/acrylate copolymer *2 3.0 parts by weight 4. Pearl pigment *3 2.0 parts by weight 5. Oil-including silicone elastomer 25 parts by weight particles according to the present embodiment 6. Talc 25 parts by weight Phase B 7. Silicone film forming agent *4 5.0 parts by weight 8. Ethylhexyl methoxysilicic acid 5.0 parts by weight 9. Octocrylene 2.0 parts by weight 10. Dimethicone *5 6.0 parts by weight 11. Preservatives Suitable amount 12. Fragrance Suitable amount Phase C 13. Silica silylate *6 4.0 parts by weight Phase D 14. Water Remainder 15. Propylene glycol 2.0 parts by weight 16. PEG-32 3.0 parts by weight *1: SI-Titan CR-50, manufactured by Miyoshi Kasei *2: SunSpheres ™ Powder, manufactured by Dow Corp. *3: Timiron Glam Silver, manufactured by Merck *4: SH200 2cs, manufactured by Toray Dow Corning Co. *5: FC5002ID Resin Gum, manufactured by Toray Dow Corning Co. *6: VM-2270 Aerogel Fine Particles, manufactured by Toray Dow Corning Co.
[0281] (Method of Preparation)
[0282] Phase A is mixed.
[0283] Phase B is mixed.
[0284] Phase A and phase B are mixed (phase AB).
[0285] Phase D is mixed.
[0286] Phase C and phase D are mixed (phase CD).
[0287] Phase AB and phase CD, above, are mixed.
[0288] Preparation 14: Mousse Blush
[0289] (Ingredients)
TABLE-US-00017 Phase A Vaseline 10 parts by weight Microcrystalline wax 5.0 parts by weight Silicone wax *1 4.0 parts by weight Phenyl trimethicone *2 8.0 parts by weight Phase B Titanium oxide *3 3.0 parts by weight Oil-including silicone elastomer 8.0 parts by weight particles according to Embodiment 6 Silica silylate *4 0.5 parts by weight Silicone dispersing agent *5 1.0 parts by weight Carmine 5.5 parts by weight 10. Titanium oxide *6 10 parts by weight Phase C 11. Silicone film forming agent *7 10 parts by weight 12. Cross-linked silicone gel *8 10 parts by weight Phase D 13. Caprylyl methicone *9 5.0 parts by weight 14. Dimethicone *10 10 parts by weight 15. Fragrance Suitable amount 16. Preservatives Suitable amount *1: 580 Wax, manufactured by Toray Dow Corning Co. *2: SH556, manufactured by Toray Dow Corning Co. *2: Eusolex T-S, manufactured by Merck *4: VM-2270 Aerogel Fine Particles, manufactured by Toray Dow Corning Co. *5: ES-5300 Formulation Aid, manufactured by Toray Dow Corning Co. *6: SI-Titan CR-50, manufactured by Miyoshi Kasei *7: FC5002ID Resin Gum, manufactured by Toray Dow Corning Co. *8: EL-7040 Hydro Elastomer Blend, manufactured by Toray Dow Corning Co. *9: FZ-3196, manufactured by Toray Dow Corning Co. *10: SH200 2cs, manufactured by Toray Dow Corning Co.
[0290] (Method of Preparation)
[0291] Phase A is heated to 75° C.
[0292] Phase B is mixed.
[0293] Phase C is mixed.
[0294] Phase C is added to phase B, and heated to 75° C. (Phase BC)
[0295] While agitating phase BC, phase A is added slowly. (Phase ABC)
[0296] Phase D is added to phase ABC (mixture), and agitated until uniform.
Preparation 15: Eyeshadow
[0297] (Ingredients)
TABLE-US-00018 Phase A Oil-including silicone elastomer particles 5.0 parts by weight according to Embodiment 6 Ba sulfate 6.0 parts by weight Zinc stearate 0.2 parts by weight Talc 62.6 parts by weight Basic magnesium carbonate *1 1.2 parts by weight Titanium oxide *2 1.8 parts by weight Preservatives Suitable amount Phase B Red no. 7 15 parts by weight Phase C Octyldodecyl myristate 2.0 parts by weight Triisostearate PEG-6 *2 1.0 parts by weight Stearic acid 2.0 parts by weight Cross-linked silicone gel *3 1.5 parts by weight Silicone film forming agent *4 1.5 parts by weight *1: Basic magnesium carbonate, manufactured by Merck *2: SI-Titan CR-50, manufactured by Miyoshi Kasei *3: 9041 Silicone Elastomer Blend, manufactured by Toray Dow Corning Co. *4: FC5002ID Resin Gum, manufactured by Toray Dow Corning Co.
[0298] (Method of Preparation)
[0299] Phase A is mixed.
[0300] Phase B is added to phase A and agitated. (Phase AB)
[0301] Phase C is heated to 75° C., added to phase AB, and agitated until uniform.
[0302] Transferred to a container and compressed.
[0303] [Aqueous Suspension of Oil-Including Silicone Elastomer]
[0304] In Preparation 16 through Preparation 18, below, rather than removing the water content in the Embodiments 1 through 7, described above, the uniform aqueous suspensions of the oil-including silicone elastomer particles according to each of the embodiments, obtained in the manufacturing processes thereof, are used as-is as cosmetic raw materials.
Preparation 16: O/W Foundation Cream
(Ingredients)
[0305]
TABLE-US-00019 Phase A Silicone emulsifier premix *1 3.0 parts by weight Cross-linked silicone gel *2 25 parts by weight Dimethicone *3 2.0 parts by weight Phenyl trimethicone *4 2.0 parts by weight Tris (caprylic/capric acid) glyceryl 3.0 parts by weight Squalane 5.0 parts by weight Jojoba oil 3.0 parts by weight Pearl pigment *5 2.0 parts by weight Phase B Water Remainder 10. Glycerin 5.0 parts by weight 11. Preservatives Suitable amount 12. Aqueous suspension of oil- 5.0 parts by weight including silicone elastomer according to the present embodiment 13. Sodium hyaluronate 1% aqueous 10 parts by weight solution *1: RM 2051 Thickening Agent, manufactured by Toray Dow Corning Co. *2: 9041 Silicone Elastomer Blend, manufactured by Toray Dow Corning Co. *3: SH200C 6cs, manufactured by Toray Dow Corning Co. *4: SH556, manufactured by Toray Dow Corning Co. *5: TIMIRON SPLENDID RED, manufactured by Merck
[0306] (Method of Preparation)
[0307] Phase A is mixed.
[0308] Phase B is mixed.
[0309] While agitating phase A, phase B is added slowly.
Preparation 17: 0/W Skin Cream
[0310] (Ingredients)
TABLE-US-00020 Phase A 1. Stearic acid 1.0 parts by weight 2. Polysorbate 80 1.2 parts by weight 3. Sorbitan sesquioleate 0.5 parts by weight 4. Glycerin stearate 1.5 parts by weight 5. Cetearyl alcohol 1.5 parts by weight 6. Dimethicone *1 5.0 parts by weight 7. Squalane 5.0 parts by weight 8. lsotridecyl isonononate 5.0 parts by weight 9. Tris (caprylic/capric acid) glyceryl 5.0 parts by weight Phase B 10. Water Remainder 11. Butylene glycol (BG) 8.0 parts by weight 12. Sodium hydroxide Suitable amount Phase C 13. Carbomer *2 0.12 parts by weight 14. Water 10 parts by weight Phase D 15. Aqueous suspension of oil-including silicone 7.0 parts by weight elastomer according to the present embodiment *1: SH2000 6cs, manufactured by Toray Dow Corning Co. *2: Carbopol 980, manufactured by Lubrizol
[0311] (Method of Preparation)
[0312] Phase A is heated to 70° C.
[0313] Phase B is heated to 70° C.
[0314] While agitating phase A, phase B is added slowly. (Phase AB)
[0315] Phase C and phase D are added to phase A, agitated until uniform, and then cooled to room temperature.
Preparation 18: O/W All-in-One Gel
[0316] (Ingredients)
TABLE-US-00021 Phase A 1. Silicone emulsifier *1 0.5 parts by weight 2. Dimethicone *2 1.0 part by weight 3. Jojoba oil 1.0 part by weight 4. Cyclopentasiloxane *3 2.0 parts by weight Phase B 5. Water Remainder 6. Glycerin 10 parts by weight 7. (Acrylate/alkyl acrylate (C10-30)) 0.2 parts by weight cross-polymer*4 8. Triethanol amine (TEA) Suitable amount 9. Preservatives Suitable amount 10. Aqueous suspension of oil- 5.0 parts by weight including silicone elastomer according to the present embodiment *1: ES-5373 Formulation Aid, manufactured by Toray Dow Corning Co. *2: SH200C 6cs, manufactured by Toray Dow Corning Co. *3: SH245 Oil, manufactured by Toray Dow Corning Co. *4: Carbopol Ultez20 Polymer, manufactured by Lubrizol
[0317] (Method of Preparation)
[0318] Phase A is mixed.
[0319] Phase B is mixed.
[0320] While agitating phase B, phase A is added slowly.
Preparation 19: Lip Stain
[0321] (Ingredients)
TABLE-US-00022 Phase A Silica silylate *1 1.5 parts by weight Hydrogenated polyisobutene *2 10 parts by weight Phase B Silicone resin wax *3 3.0 parts by weight Beeswax 4.5 parts by weight Preservatives Suitable amount Phase C Titanium oxide *4 7.7 parts by weight Red No. 201 lake *5 2.75 parts by weight Red no. 202 *6 2.75 parts by weight Phase D Caprylyl methicone *7 10 parts by weight Silicone dispersing agent *8 2.0 parts by weight Phase E 11. Barium sulfate 0.2 parts by weight 12. Oil-including silicone elastomer 2.0 parts by weight particles according to the present embodiment Phase F 13. Clay minerals *9 7.0 parts by weight 14. Antioxidants Suitable amount 15. lsododecane 15 parts by weight 16. Dimethicone *10 10 parts by weight 17. Silicone film forming agent *11 20 parts by weight 18. Ethylene/octene copolymer. *12 0.5 parts by weight 19. Fragrance Suitable amount *1: VM-2270 Aerogel Fine Particles, manufactured by Toray Dow Corning Co. *2: Pearleme 4, manufactured by NOF Corp. *3: SW-8005 C30 Resin Wax, manufactured by Toray Dow Corning Co. *4: Unipure White LC 987 AS-EM, manufactured by Sensient *5: Unipure Red LC 304, manufactured by Sensient *6: Unipure Red LC 3079, manufactured by Sensient *7: SS-3408, manufactured by Toray Dow Corning Co. *8: ES-5300 Formulation Aid, manufactured by Toray Dow Corning Co. *9: Bentone Gel (R) ISDV, manufactured by Elementis *10: SH200 1.5cs, manufactured by Toray Dow Corning Co. *11: 749 Fluid, manufactured by Toray Dow Corning Co. *12: EcoSmooth ™ Delight H, manufactured by Dow Chemical
[0322] (Method of Preparation)
[0323] Phase A is mixed.
[0324] After melting phase B through heating to 80° C. and then cooling to 60° C., phase A is added and agitated. (Phase AB)
[0325] Phase C is agitated until uniform.
[0326] Phase C and phase D are mixed. (Phase CD)
[0327] Phase CD is added to phase AB, above, and agitated at 60° C. (Phase ABCD)
[0328] Phase E is added to phase ABCD, above, and agitated. (Phase ABODE)
[0329] Phase F is added to phase ABCDE, above, agitated, and cooled to no higher than 40° C.
Preparation 20: Face Powder
[0330] (Ingredients)
TABLE-US-00023 Phase A Talc *1 75 parts by weight Sericite *2 10 parts by weight Zinc oxide *3 5.0 parts by weight Magnesium stearate 4.0 parts by weight Oil-including silicone elastomer particles 5.0 parts by weight according to the present embodiment Phase B 6. Squalane 1.0 part by weight *1: SI-talc, manufactured by Miyoshi Kasei *2: SI-sericite FSE, manufactured by Miyoshi Kasei *3: FINEX-30-OTS, manufactured by Sakai Chemical Industry Co.
[0331] (Method of Preparation)
[0332] Phase A is mixed.
[0333] Phase B is added to phase A, and agitated until uniform.
Preparation 21: Hair Chalk
[0334] (Ingredients)
TABLE-US-00024 Phase A Talc 63.7 parts by weight Magnesium stearate 3.0 parts by weight Methyl paraben 0.2 parts by weight Propyl paraben 0.1 parts by weight Oil-including silicone elastomer particles accordingt o the present embodiment 5.0 parts by weight Titanium oxide *1 5.0 parts by weight Phase B 7. Red No. 202 *2 15 parts by weight Phase C Cross-linked silicone gel *3 8.0 parts by weight *1: Unipure White LC 987 AS-EM, manufactured by Sensient *2: Unipure Red LC 3079, manufactured by Sensient *3: 9041 Silicone Elastomer Blend, manufactured by Toray Dow Corning Co.
[0335] (Method of Preparation)
[0336] Phase A is mixed.
[0337] Phase B is added and mixed.
[0338] Phase C is added and mixed.
[0339] Transferred to a container and compressed.
[Potential for Use in Industry]
[0340] When compared to the known silicone particles or oil-including silicone particles, the oil-including silicone particles according to the present invention have low oil absorption, and suppress agglomeration with the passage of time, and thus have superior storage stability, ease of handling, and mixture stability, and can be mixed easily as additives, and when mixed into cosmetics as cosmetic raw materials, can improve the feel, and thus can be used in skin cosmetics, makeup, and the like. Moreover, taking advantage of the physical properties thereof, the oil-including silicone elastomer particles according the present invention can be used also as an additive for thermally curable resin compositions, thermoplastic resin compositions, and the like, as an application for electronic materials, or as a surface lubricant for plastic films.