JPH09291215A - Silicone resin emulsion composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain the subject composition in which emulsified particles are uniform, excellent in preservation stability and useful for cosmetics, etc., by dispersing polyorganosilsesquioxane powder with polyorganosiloxane in water by using a surfactant. SOLUTION: This silicone resin emulsion composition contains (A) 10-60wt.% of polyorganosiloxane and (B) 0.1-50wt.% of powdery polyorganosilsesquioxane in an emulsion system. The component B is preferably spherical powder having 0.1-100μm particle size. The composition is obtained by mixing the component A with the component B, adding (C) a surfactant to the mixture, then adding water and emulsifying each component by high shearing force. The amount of the component C to be added is 1-20wt.%, preferably 5-15wt.% based on the composition.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a silicone resin emulsion composition, and more specifically, it contains a polyorganosilsesquioxane powder in emulsified particles, has uniform emulsified particles, and is excellent in storage stability. / W type silicone resin emulsion composition. The present invention also relates to cosmetics and polishes obtained by blending the above silicone resin emulsion composition.

[0002]

2. Description of the Related Art Silicone resins have been conventionally used for heat resistance,
Due to its excellent weather resistance and water resistance, it is used in heat- and weather-resistant paint vehicles and coating agents for the purpose of water repellency, antifouling, and mold release, and also has an excellent feel and good gloss. It is also used in hair cosmetics and the like to impart slipperiness.

It is also widely known to use polymethylsilsesquioxane powder together for these purposes. But,
Since polymethylsilsesquioxane powder is originally highly hydrophobic, it is difficult to satisfactorily disperse it in an aqueous emulsion system such as an emulsion. Moreover, since the compounding amount of the polymethylsilsesquioxane powder is limited, the resulting emulsion composition may not be able to sufficiently impart the characteristics possessed by the powder, and even if it can be dispersed in the system, the powder can be dispersed over time. Precipitates and a stable emulsion system cannot be obtained.

For example, a water / oil repellent composition containing a ladder polymer of polyorganosilsesquioxane (JP-A-63-146976 and JP-A-1-95181).
(See Japanese Patent Laid-Open Publication No. Heisei No. 1993), and hair cosmetics containing polymethylsilsesquioxane powder (see Japanese Laid-Open Patent Publication No. 5-310533), but when the system is an emulsion system, dispersion is difficult, There is a problem that sufficient characteristics cannot be obtained due to sedimentation over time. Further, as a method for producing a polyorganosilsesquioxane emulsion, a method of emulsifying a corresponding raw material organosilane in the presence of a cationic surfactant, and then polycondensing the emulsified organosilane with an alkaline condensation catalyst ( JP-A-62-43
No. 424) is disclosed, the emulsification for polycondensation is emulsification with only a cationic surfactant,
There is a restriction that the obtained emulsion cannot be mixed with an anionic emulsion. Furthermore, the emulsion thus obtained is not satisfactory because unreacted organosilane remains, so that it may cause reaction, aggregation, precipitation, etc. when compounded with other materials. . Further, a polishing agent to which polymethylsilsesquioxane powder is added (see JP-A-61-159474) has been proposed. However, since the powder is directly added to the system, dispersibility of the powder in the polishing agent is proposed. However, it was not satisfactory because it may cause aggregation and sedimentation.

[0005]

SUMMARY OF THE INVENTION The object of the present invention is to obtain an O / O emulsion having uniform emulsion particles, improved dispersibility of the polyorganosilsesquioxane powder in the emulsion system, no sedimentation and excellent storage stability. A W-type emulsion composition is provided. Another object of the present invention is to provide a hair cosmetic composition and a polish composition obtained by blending such an emulsion composition.

[0006]

Means for Solving the Problems As a result of repeated studies to achieve the above object, the present inventors have found that polyorganosilsesquioxane powder is added to water together with polyorganosiloxane by using a surfactant. The present invention has been completed by finding that an emulsion composition containing the powder in emulsified particles and having good characteristics can be obtained by dispersing the particles.

That is, the present invention provides a composition comprising (A)
Polyorganosiloxane 10 to 60% by weight and (B) polyorganosilsesquioxane powder 0.1 to 5
0% by weight in the emulsified particle system, O /
W type silicone resin emulsion composition,
The present invention relates to cosmetics and polishes obtained by blending the silicone resin emulsion composition thus obtained.

[0008]

BEST MODE FOR CARRYING OUT THE INVENTION The polyorganosiloxane of the component (A) used in the present invention not only imparts gloss and slipperiness to the composition and imparts moist luster to hair and substrate, It is a component for holding the component (B) described below in the oil phase particle system of the O / W type emulsion.
The component (A) basically has a linear siloxane skeleton, and may have some branching, and it is preferable that the whole molecule has a linear structure.

Examples of the organic group bonded to a silicon atom in the molecule include alkyl groups such as methyl, ethyl, propyl, butyl and hexyl; cycloalkyl groups such as cyclohexyl; alkenyl groups such as vinyl and allyl; phenyl, tolyl and the like. An aryl group; and a group in which a hydrogen atom bonded to a carbon atom of these groups is substituted with a halogen atom, a cyano group, an amino group or the like, for example, a chloromethyl group, 3,
3,3-trifluoropropyl group, cyanomethyl group, 3
-Aminopropyl group and the like are exemplified. As the other group bonded to the silicon atom, an alkoxy group, a hydroxyl group, a hydrogen atom and the like may be partially contained. Among these, a methyl group is particularly preferable because the obtained composition has good stability, glossing effect, slipperiness, and the like, and is inexpensive in cost. That is, polydimethylsiloxane is preferable as the polyorganosiloxane. Incidentally, as the terminal group of the molecular chain, a triorganosilyl group,
Alternatively, a group in which a hydroxyl group is bonded to a silicon atom instead of a part of the organic group is exemplified. As such component (A), a polydiorganosiloxane end-capped with a trimethylsilyl group or a dimethylhydroxysilyl group is preferable, and a polydimethylsiloxane end-capped with a trimethylsilyl group is particularly preferable.

The polyorganosiloxane as the component (A) is generally soluble in an organic solvent and has a viscosity at 25 ° C. of 10 to 100,000,000 cP, which is called a silicone oil or a silicone raw rubber. Is used. When used in combination with the polymethylsilsesquioxane powder of the component (B), an emulsion composition having good stability without sedimentation of the powder can be obtained, and thus the viscosity at 25 ° C. is 10, 0
00 to 10,000,000 cP is preferable, and 5
Particularly preferred is one having a viscosity of 50,000 to 5,000,000 cP.

The amount of component (A) blended is 10 to 60% by weight, preferably 20 to 40% by weight of the emulsion composition of the present invention.
% By weight. If it is less than 10% by weight, the emulsion is likely to separate during storage, and the effects of the component (A) such as gloss and slipperiness imparted to the composition are not sufficient. The effect of holding in the system cannot be obtained. On the other hand, if it exceeds 60% by weight, it is difficult to emulsify, and it tends to be inverted during storage to increase the apparent viscosity of the system, which makes it difficult to handle.

The polyorganosilsesquioxane powder of the component (B) used in the present invention is a resin having a three-dimensional siloxane structure composed of monoorganosilsesquioxane units, which is condensed with a trifunctional hydrolyzable silane. -It is a cured product obtained by polymerization, is a powder that is infusible, has no softening point, and is generally insoluble in organic solvents. When the obtained emulsion composition is used in cosmetics, it gives excellent feel, slipperiness, etc., and when used in a polish, it can impart good polish, water repellency, workability, etc., The component (B) is preferably spherical, and particularly spherical. In addition, the emulsion composition is excellent in stability, and the powder is not settled, and the composition is satisfactorily provided with the above-mentioned characteristics. Therefore, the average particle diameter of the powder is 0.1 to 10
It is preferably 0 μm, and particularly preferably 0.3 to 20 μm.

Examples of the organic group bonded to the silicon atom include alkyl groups such as methyl, ethyl, propyl, butyl, octyl, lauryl and stearyl; alkenyl groups such as vinyl and allyl; aryl groups such as phenyl, tolyl and naphthyl; 2 -Aralkyl groups such as phenylethyl; cycloalkyl groups such as cyclopentyl and cyclohexyl; or these groups are glycidyloxy groups, oxolane oxygen, amino groups, methacryloxy groups, carboxyl groups, cyano groups, polyoxyalkylene groups, mercapto groups, hydroxy groups. A monovalent group substituted with a group is exemplified. Among these, when the obtained emulsion composition is used for cosmetics, it gives excellent feel, slipperiness, etc., and when it is used for a polish, it gives good polish, water repellency, workability, etc. An unsubstituted alkyl group and a phenyl group are preferable, and a methyl group is particularly preferable because they can be imparted.

Also, those treated with various surface treatment agents can be used depending on the purpose. As the surface treatment agent, a treatment agent for imparting water repellency such as fluoroalkylalkoxysilanes, alkylalkoxysilanes, and hexamethyldisilazane; or an epoxy group, an amino group,
A treatment agent for imparting hydrophilicity and / or carbon functionality, such as alkoxysilanes having an alkyl group substituted with a methacryloxy group, a carboxyl group, a cyano group, a polyoxyalkylene group, a mercapto group, a hydroxy group, etc. It is illustrated. Since the cosmetics and polishes containing the resulting emulsion composition have good properties, the untreated ones or the ones treated with a water repellent treatment are preferable. When it is used by being mixed with a material or a polish, an untreated one is particularly preferable.

As a method for producing such component (B), a method is known in which an organotrialkoxysilane such as methyltrimethoxysilane or methyltriethoxysilane is hydrolyzed and condensed using an alkali catalyst. (JP-A-54-72300, JP-A-60-13)
813, JP-A-63-77940, JP-A-63-295637 and JP-A-1-21703.
It is preferable to perform hydrolysis / condensation using ammonia or amines as a catalyst, since uniform and spherical particles having few impurities are obtained.

The amount of component (B) blended is 0.1 to 50% by weight, preferably 0.2 to 50% by weight of the emulsion composition of the present invention.
It is 10% by weight. If it is less than 0.1% by weight, good properties cannot be obtained when the resulting emulsion composition is blended in cosmetics and polishes, and if it exceeds 50% by weight,
This is because the stability of the obtained emulsion composition is reduced. Further, the amount of the component (B) is preferably 10 to 70 parts by weight based on 100 parts by weight of the component (A) in order to obtain an emulsion composition having good stability.
20 to 50 parts by weight are particularly preferred.

The silicone resin emulsion composition of the present invention comprises the above component (A), and optionally the component (B) dispersed in an oil phase containing an organic solvent, as emulsion particles in the aqueous phase. It is a dispersed O / W type silicone resin emulsion composition. In order for the composition of the present invention to form such an O / W type emulsion, another component (C) is used.
And the water of the component (D) are used, and if necessary, an organic solvent is used.

The surfactant as the component (C) functions to uniformly disperse the component (A) and the component (B) in water and improve the storage stability of the obtained emulsion. As such a surfactant, any of a nonionic surfactant, an anionic surfactant and a cationic surfactant may be used.

Examples of nonionic surfactants include glycerin fatty acid esters such as glyceryl monolaurate, glyceryl monomyristate, glyceryl monostearate and glyceryl monooleate; polyglycerin fatty acid esters having similar fatty acid residues, sorbitan fatty acid. Esters, polyoxyethylene glycerin fatty acid esters, polyoxyethylene sorbitan fatty acid esters and polyoxyethylene fatty acid esters; polyoxyethylene lauryl ether, polyoxyethylene cetyl ether, polyoxyethylene stearyl ether, polyoxyethylene oleyl ether Ethylene alkyl ether; such as polyoxyethylene octyl phenyl ether, polyoxyethylene nonyl phenyl ether Polyoxyethylene alkyl phenyl ethers; polyoxyethylene-oxypropylene block copolymer; as well as polyether-modified polydimethylsiloxane is illustrated.

Examples of the anionic surfactant include alkylbenzenes such as sodium hexylbenzenesulfonate, sodium octylbenzenesulfonate, sodium decylbenzenesulfonate, sodium dodecylbenzenesulfonate, sodium cetylbenzenesulfonate and sodium myristylbenzenesulfonate. Sodium sulfonate; sodium alkylnaphthyl sulfonate such as sodium butylnaphthyl sulfonate; sodium polyoxyethylene octyl ether sulfate,
Polyoxyethylene monoalkyl ether sulfate sodium salt such as sodium polyoxyethylene decyl ether sulfate and sodium polyoxyethylene icosyl ether sulfate; polyoxyethylene mono (alkyl) sodium salt such as sodium polyoxyethylene decyl phenyl ether sulfate Examples thereof include phenyl) ether sulfate sodium salt.

As the cationic surfactant, octyltrimethylammonium chloride, dodecyltrimethylammonium chloride, hexadecyltrimethylammonium chloride, tallow trimethylammonium chloride, coconut oil trimethylammonium chloride, octyldimethylbenzylammonium chloride, decyldimethylbenzylammonium chloride, Examples are quaternary ammonium salts such as dioctadecyldimethylammonium chloride.

These surfactants are usually used in combination of two or more of the same system or different systems so that a good emulsion can be easily obtained, and in combination with other emulsions or in other emulsions. Nonionic surfactants are preferable because they can be used in combination.

The content of the component (C) is usually 1 to 20% by weight, preferably 5 to 15% by weight of the emulsion composition of the present invention. When it is less than 1% by weight, it becomes difficult to disperse each component in the obtained emulsion composition well, and when it exceeds 20% by weight, the stability of the obtained emulsion composition with time decreases.

The component (D) is water, which is a dispersion medium for obtaining a uniform emulsion composition by dispersing or dissolving the components (A), (B) and other components. The blending amount of the component (D) is preferably 20 to 80% by weight, particularly preferably 30 to 60% by weight, based on the emulsion composition of the present invention.

In the present invention, an organic solvent may be added, if necessary, in order to dissolve the component (A), assist the dispersion of the component (B) in the oil phase, and facilitate the emulsification. The organic solvent is not particularly limited as long as it fulfills the above functions, and n-hexane, n-heptane, cyclohexane, methylcyclohexane, isoparaffin mixed solvent, gasoline, rubber volatile oil, mineral spirits, aliphatic oil such as kerosene. Hydrocarbons; aromatic hydrocarbons such as toluene and xylene; ethers such as n-butyl ether and methylphenyl ether; ketones such as methyl isobutyl ketone and diethyl ketone; acetic acid-n-butyl, isononyl isononanoate , Isotridecyl isononanoate, isopropyl laurate, isopropyl myristate, dioctanoic acid-2,2-dimethylpropene-
Esters such as 1,3-diyl; chain volatile siloxanes such as hexamethyldisiloxane, octamethyltrisiloxane, decamethyltetrasiloxane, dodecamethylpentasiloxane; and octamethylcyclotetrasiloxane, decamethylcyclo Cyclic volatile siloxanes such as pentasiloxane and dodecamethylcyclohexasiloxane are exemplified, and they are appropriately selected depending on the application, and one kind may be used or two or more kinds may be used in combination. Of these, it is preferable to use aliphatic hydrocarbons or esters because they can favorably emulsify the components (A) and (B), and particularly selected from such aliphatic hydrocarbons and esters. When the composition containing at least one organic solvent is added to hair cosmetics such as shampoos, rinses, and hair conditioners, a characteristic of giving a smooth and good feel to the hair after use is obtained.

The content of the organic solvent is usually 0 to 60% by weight of the emulsion composition of the present invention, preferably 5%.
３０30% by weight. If it exceeds 60% by weight, the stability of the resulting emulsion composition with time decreases.

Preservatives, thickeners and the like can be added to the composition of the present invention, if necessary. Examples of preservatives include methyl p-hydroxybenzoate, propyl p-hydroxybenzoate, sodium benzoate, citric acid and salicylic acid. Examples of the thickener include alginic acid, gum arabic, casein, methyl cellulose, hydroxyethyl cellulose, cation-modified etherified cellulose, hydroxypropylden powder, polyvinyl alcohol, polyvinylpyrrolidone and bentonite.

The silicone resin emulsion composition of the present invention can be manufactured by a manufacturing method including the following steps. That is: (1) mixing component (A) and component (B); (2) mixing component (C) with the mixture obtained in step (1); (3) next step (2) ) To the mixture obtained in
Is added, high shear force is applied to disperse each component, and the mixture is emulsified. These steps may be carried out continuously, or each step may be carried out independently. In the latter case, when precipitation of component (B) or separation of each component is observed, remixing is performed. Then, it is preferable to proceed to the next step.

The mixing in step (1) and step (2) is usually at a temperature of 40 to 90 ° C., preferably 60 to 80 ° C., and the system is usually less than 500 rpm, preferably 10 to 60 rp.
A paddle type, anchor type, gate type, etc. paddle type mixer; a propeller type mixer; a planetary mixer or other low speed stirring device is used to give rotation of m.
It is performed by stirring for 0.5 to 10 hours, preferably 1 to 4 hours through both steps until the blended components are uniformly dispersed.

The addition and emulsification of water in the step (3) are carried out under a high shearing force, usually at 20 to 90 ° C., preferably 30 to 70.
It is carried out at a temperature of 0 ° C., usually for 0.5 to 8 hours, preferably 1 to 4 hours. The high shearing force required for emulsification can be given by using a high-speed shearing dispersing device such as a colloid mill, a homomixer, a homodisper, a flow jet mixer, an ultramixer; or a high-pressure shearing dispersing device such as a homogenizer. When using a high speed shear disperser, the rotation speed is 500 to 10,000 rp
m is preferable, and 1,000 to 5,000 rpm is particularly preferable. If it is less than 500 rpm, an emulsion having good stability cannot be obtained, and if the number of rotations is more than 10,000 rpm, the emulsion formed is rather destroyed. On the other hand, when a high-pressure shear disperser is used, it is usually 50 to 1,000.
kgf / cm ^2, preferably under a pressure of 100~500kgf / cm ^2, passing the mixture through a gap.

Steps (1) to (3) can be carried out by a series of operations in one apparatus using an apparatus in which a low speed stirring apparatus and a high shearing force dispersing apparatus are combined. In (2), high shear dispersion may be used in combination with low speed stirring. Examples of such a device include an Aji-homomixer combining an anchor mixer and a homomixer; a dispersing device combining a planetary mixer and a homodisper; a dispersing device such as a combimix combining an anchor mixer, a homomixer and a homodisper. To be The use of such a dispersing device is preferable since an emulsion composition having excellent storage stability can be obtained. Further, a high-pressure shearing dispersion device may be used together before, after or during the above series of operations, preferably after the operations.

The silicone resin emulsion composition can be prepared as described above. Furthermore, if necessary, the composition thus obtained can be diluted with (D) water to obtain an O / W type emulsion composition having a desired silicone concentration. This dilution step does not require the application of high shear forces.

The O / W type emulsion obtained by the production method of the present invention has an average particle size of the oil phase of about 0.1 to 1 although it varies depending on the average particle size of the component (B) used.
It is 00 μm. When powder having an average particle size of 1 μm or less is used as the component (B), the average particle size of the oil phase is 1.0
Easy to obtain emulsion of ~ 2.0μm, while 2μm
When the above powders are used, the average particle size of the powder is 0.
It is easy to obtain an emulsion having an average particle size as large as 1 to 0.5 μm. From this, the oil phase particles in the emulsion of the present invention have a form in which the surfaces of the particles of component (B) are covered with the polyorganosiloxane of component (A), and the surfaces of this component (B) are covered. It is judged that the surfactant is oriented in the component (A), and the emulsion is thereby stabilized.

Among the average particle diameters of the oil phase of the above emulsion, when the emulsion of the present invention is used by being mixed with a cosmetic, a good feeling in use can be obtained, so that the average particle diameter is 0.3. It is preferable to use an emulsion having an average particle size of 0.3 to 50 μm, and when it is used as a polish, it has an average particle size of 0.3 to 50 because of its excellent workability.
It is preferable to use a μm emulsion.

[0035]

The emulsion composition of the present invention is an O / W type emulsion containing the polyorganosilsesquioxane powder of component (B) in the emulsified particle system which is the oil phase. It is characterized in that it has good storage stability without sedimentation of B) over time. The dispersion obtained by simply dispersing the component (B) in water without using the polyorganosiloxane of the component (A) of the present invention is a good dispersion of the component (B) in the system. It is difficult to carry out the process, and the component (B) precipitates over time, resulting in insufficient storage stability. Moreover, since the emulsion composition of the present invention is an O / W type emulsion,
When used as a cosmetic, a good feeling without stickiness is obtained, and when used as a polish,
Excellent workability when applying and wiping.

Due to such characteristics, the silicone resin emulsion composition of the present invention can be used for cosmetics such as hair cosmetics, skin cosmetics, makeup cosmetics and cleansing agents; automobile bodies, tires, furniture, leather products, office work. It is useful as a raw material for polishes for various purposes including equipment; various coating agents; release agents. Particularly when blended in a cosmetic composition, an excellent feel is obtained, and particularly when used in a hair cosmetic composition, a good gloss is obtained, and when blended in a polish, good gloss and excellent workability are obtained. There are advantages.

[0037]

EXAMPLES The present invention will be described below with reference to Examples and Comparative Examples. In these examples, “part” means “part by weight”, “%” means “% by weight”, and the viscosity means a value at 25 ° C. The present invention is not limited by these examples.

Examples 1 to 3 Preparation and Evaluation of Silicone Resin Emulsion Composition A stainless steel container has a stator on its central axis and rotates around it to scrape off the contents adhering to the vessel wall. An emulsifying device (Ajihomo Mixer, Special Machine Co., Ltd.) in which an anchor-type rotary low-speed stirring device a having a stirring section equipped with a high speed shearing dispersion device b (homomixer) provided inside the stator is combined. (Commercial name) and the composition and composition ratio shown in Table 1
A W type silicone resin emulsion composition was prepared.

That is, first, 25.0 parts of polydimethylsiloxane shown in Table 1 and isoparaffin mixed solvent 16.
5 parts and 8.5 parts of polymethylsilsesquioxane powder of each average particle size were charged, the temperature in the container was raised to 70 ° C., the stirring device a was 40 rpm, and the stirring device b was 1,000 rp.
The mixture was rotated to m 3 and stirred and mixed for 3 hours to dissolve the polydimethylsiloxane in the isoparaffin mixed solvent and uniformly disperse the polymethylsilsesquioxane powder. Then, 3.4 parts of polyoxyethylene (4) lauryl ether and 3.4 parts of polyoxyethylene (23) lauryl ether were added, and stirring was continued at 70 ° C. for 2 hours to homogenize the system. Then add 4.0 parts of water and
The mixture was stirred for a period of time to invert the phase to form a transparent grease. After stopping the stirrer b, 22.5 parts of water and 0.085 part of salicylic acid were added while rotating the stirrer a at 40 rpm,
The mixture was stirred for 1 hour to obtain uniform O / W type emulsion compositions E-1 to E-3 having a silicone concentration of 40%.

The average particle size of the oil phase particles of the obtained emulsion was measured with a particle size measuring device LS-100Q (Coulter,
It was measured by the product name). In addition, the stability of the emulsion was evaluated by observing the presence or absence of polymethylsilsesquioxane powder precipitated at the bottom by a centrifugation stability test and a storage stability test. The results are shown in Table 1.

Example 4 Preparation and Evaluation of Silicone Resin Emulsion Composition A planetary mixer type low speed stirring device c having two rotary stirring blades, and a stirring device c provided between them so as not to come into contact with the stirring device c and having teeth on the periphery thereof. Using a high-speed agitator d (homodisper) having a disk with upper and lower mold protrusions alternately provided in the same stainless steel container (Hibis Dispermix, trade name of Tokushu Kika Co., Ltd.) An O / W type silicone resin emulsion composition was prepared with the components and composition ratios shown in 1.

That is, first, 25.0 parts of polydimethylsiloxane shown in Table 1 and isoparaffin mixed solvent 16.
Charge 5 parts and 8.5 parts of polymethylsilsesquioxane, raise the temperature in the container to 70 ° C., and stir the device c at 20 rpm.
The stirring device d was rotated at 1,000 rpm and stirred for 3 hours to dissolve polydimethylsiloxane in isoparaffin and uniformly disperse polymethylsilsesquioxane. Then, 3.4 parts of polyoxyethylene (4) lauryl ether and 3.4 parts of polyoxyethylene (23) lauryl ether were added, and the mixture was further stirred at 70 ° C. for 2 hours to make the system uniform. Further, 4.0 parts of water was added, and the mixture was stirred for 3 hours to invert the phase to form a transparent grease. After stopping the stirrer d, 22.5 parts of water and 0.085 part of salicylic acid were added, the stirrer c was rotated at 20 rpm and stirred for 1 hour to obtain a uniform O / concentration of 40% of silicone concentration.
W-type emulsion composition E-2 was obtained.

The average particle size of the oil phase particles of the obtained emulsion was measured by the same device as in Examples 1-3.
In addition, the stability of the emulsion was evaluated by the same method as in Examples 1 to 3. The results are shown in Table 1.

[0044]

[Table 1]

As is clear from Table 1, the silicone resin emulsion composition of the present invention is extremely stable to both centrifugation at 3,000 rpm and long-term storage at 50 ° C., and polymethylsilsesquioxane. No sedimentation of powder or separation of emulsion was observed.

Examples 5 and 6, Comparative Example 1 Preparation and Evaluation of Rinse-in Shampoo Using the silicone resin emulsion compositions E-1 or E-4 prepared in Example 1 or Example 4, respectively.
The rinse-in shampoos of Example 5 and Example 6 were prepared with the components and the composition ratios shown in Table 2. For comparison, a rinse-in shampoo of Comparative Example 1 was prepared by using polydimethylsiloxane and polymethylsilsesquioxane powder instead of the silicone resin emulsion composition.

That is, among the components shown in Table 2, a surfactant, a thickener, glycerin and methyl p-hydroxybenzoate were placed in a mixing tank and mixed at 80 ° C. with stirring.
In Example 5 and Example 6, pure water was added thereto, and the mixture was cooled to 30 ° C. with stirring, and then 5.0 parts of each of the above silicone resin emulsion compositions was added and mixed to form a rinse-in shampoo. Obtained. Comparative Example 1
Then, add pure water and cool to 50 ° C with stirring, then add a mixture of polydimethylsilsesquioxane powder dispersed in polydimethylsiloxane in advance, cool to 40 ° C with stirring, and compare A rinse-in shampoo was prepared for.

The stability of the rinse-in shampoo thus obtained was evaluated by a centrifugation stability test and a storage stability test as in Examples 1-3. The cosmetic properties of the rinse-in shampoo were evaluated by the average value of the evaluation points by 20 female panelists, with the smoothness at the time of use, combability after use, volume feeling, feel and gloss as evaluation items. . The results are shown in Table 2.

[0049]

[Table 2]

Examples 7 to 10 and Comparative Example 2 The silicone resin emulsion compositions E-1 to E-4 prepared in Examples 1 to 4 were used, and the components and composition ratios shown in Table 3 were used to obtain Example 7. 10 to 10 polishes were prepared. Further, for comparison, the polish agent of Comparative Example 2 was prepared by using polydimethylsiloxane and polymethylsilsesquioxane powder instead of the silicone resin emulsion composition.

That is, 25.0 parts of mineral spirit, 10.0 parts of montan oxide wax, and 1.oleic acid.
0 part and 0.8 part of morpholine were added and heated to 85 ° C. to completely dissolve it. While maintaining this mixture at 85 ° C., while stirring with a homomixer, 13.2 parts of water heated to 80 ° C. was added, and the mixture was cooled to 40 ° C. with stirring, and while continuing stirring, the above silicone resin emulsion composition was prepared. The emulsion type polish of Examples 7 to 10 was prepared by adding 5.0 parts of the product. On the other hand, in Comparative Example 2, a mixture of mineral spirit and an isoparaffin mixed solvent was used as the organic solvent, polydimethylsiloxane used in place of the silicone resin emulsion composition was used in the first step, and polymethylsilsesquioxane powder was used. An emulsion type polish was prepared in the same manner as in Examples 7 to 10 except that montan oxide wax was added next.

The stability of the resulting polish was evaluated according to Example 1
The evaluation was carried out by a centrifugation stability test and a storage stability test in the same manner as in (3). In addition, the properties of the polish were evaluated as the evaluation items such as extensibility, ease of wiping, degree of gloss increase and water repellency. The results are shown in Table 3.

[0053]

[Table 3]

As is clear from Tables 2 and 3, the rinse-in shampoo of Comparative Example 1 and the polish of Comparative Example 2 showed sedimentation of the polymethylsilsesquioxane powder, whereas the silicone of the present invention. The rinse-in shampoo and the polish which used the resin emulsion composition all showed the outstanding stability, and the characteristic was also excellent.

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Claims (6)

[Claims] 1. A composition comprising (A) 10 to 60% by weight of polyorganosiloxane, and (B) 0.1 to 50% by weight of polyorganosilsesquioxane powder in an emulsified particle system. An O / W type silicone resin emulsion composition comprising: 2. The composition according to claim 1, wherein the polyorganosilsesquioxane powder (B) is a spherical polymethylsilsesquioxane powder having a particle size of 0.1 to 100 μm. 3. A step of (1) mixing (A) and (B); (2) a step of adding (C) a surfactant to the mixture obtained in step (1); (3) a step of O / according to claim 1 or 2, which is obtained by a production method including a step of adding (D) water to the mixture obtained in (2), applying a high shearing force to disperse each component, and emulsifying the mixture. W type silicone resin emulsion composition. 4. A shearing force of 500 is applied in the step (3).
A composition according to claim 3 provided at a rotational speed of from 10,000 rpm. 5. A cosmetic obtained by blending the silicone resin emulsion composition according to any one of claims 1 to 4. 6. A polishing agent obtained by blending the silicone resin emulsion composition according to any one of claims 1 to 4.