JPH10306013A - Silicone emulsion, its production and hair cosmetic - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain the subject O/W-type emulsion having easily controllable particle diameter, a narrow particle diameter distribution and excellent emulsion stability and compounding stability in spite of large particle diameter by adding water in an amount larger than the phase-conversion volume at a stroke to a mixture of a polyorganosiloxane and a surfactant, stirring the product and diluting with the remaining part of water. SOLUTION: An emulsion having a relatively large particle diameter (e.g. 1-100 μm) difficult to get a high stability can be produced by mixing a mixture of (A) a polyorganosiloxane [e.g. a compound of the formula Ra SiO(4-a)/2 (R is a univalent hydrocarbon group; (a) is a positive number smaller than 4), etc.] and (B) a surfactant (e.g. a polyoxyethylene fatty acid ester) with 1-5 times volume of water based on the volume of water at a phase-conversion point and diluting the product by adding the remaining part of water. The amount of the component B is preferably 1-30 pts.wt. based on 100 pts.wt. of the component A.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an O / W type silicone emulsion which is used in various fields for the purpose of polishing, defoaming, releasing, slipping and improving touch, and a method for producing the same. In particular, the present invention relates to a silicone emulsion suitably used in the cosmetic / cosmetic field for the purpose of improving feel and the like, and a method for producing the same.

[0002]

BACKGROUND OF THE INVENTION Conventionally, silicone emulsions have been frequently used for the purpose of imparting a feeling of smoothness and gloss to hair and skin. In the case of imparting the characteristics of silicone, it is advantageous that the particles adhere quickly to the hair and skin and do not run off during use.Therefore, it is expected that the larger the emulsion particle diameter, the better the characteristics will be obtained. When the diameter is increased, there is a problem that the stability of the emulsion is reduced, and when blended in various products, the blending stability with them is significantly reduced. Emulsions generally have a tendency to become less stable as the particle size increases, but this tends to increase the particle size distribution when attempting to increase the particle size, and further to a particle size distribution with multiple peaks. In many cases, this is considered to have caused an extreme decrease in stability. Therefore, at present, the particle size of the silicone emulsion is 1 μm
Those having a relatively small particle diameter of less than are often used. Several methods have been known to control the emulsion particle size. For example, the type of surfactant and H
There is a method of selecting LB. In this case, in order to obtain an emulsion having a desired particle size according to the silicone used, the number of points to be examined is very high, as is clear from the large number of types of surfactants currently on the market. In many cases, there is a problem that it takes a long time to study. Conversely, in the field of cosmetics / cosmetics and the like, usable surfactants are limited, and there has been a problem that it is difficult to obtain an emulsion having sufficiently satisfactory properties only by combining these surfactants. As a specific method for controlling the particle size of the emulsion, an HLB method (Griffin, WC: J. Soc. Cosme
t.Chem., 1: 311,1949), Liquid crystal emulsification method (Washitani et al .: Oil Chemistry, 3
0,38,1981), phase inversion emulsification method (TJ Lin, J. Soc. Cosmet.
m., 30 167,976) and D-phase emulsification method (Washitani et al .: Nikka, 13
99, 1983). However, these emulsification methods are mainly for obtaining a product having a small particle size of less than 1 μm, and cannot be said to be an effective means for controlling the particle size of a product having a large particle size as in the present invention. Of course, depending on the surfactant used, particles having a particle size of 1 μm or more may be obtained, but have the above-mentioned problems such as stability. As another method of controlling the particle size, a method of changing the shear during emulsification by changing the temperature during emulsification, changing the type of emulsifier, changing the stirring speed during emulsification, or the like can be considered. However, in this method, it is difficult to accurately control the temperature and the stirring speed, and the share at the time of emulsification is never uniform throughout the emulsification system. The distribution of the particle size is widened or the particle size distribution has a plurality of peaks. This happens when,
The stability of the emulsion and the mixing stability with other materials are significantly reduced. This tendency is particularly remarkable for large particle size products. This is because the smaller the shear applied at the time of stirring, the larger the particle size of the emulsion, but it is difficult to uniformly apply a small shear to the whole. Also,
In actual production, the larger the production scale, the more difficult it is to give a uniform share to the entire emulsification system.In addition, when the production equipment changes or the scale changes, the conditions such as temperature and rotation speed are the same. Even so, there are many cases where the particle diameters are different, and there has been a problem that it is necessary to examine the manufacturing conditions such as the optimum temperature and the number of revolutions each time.

[0003]

An object of the present invention is to solve the above problems,
An object of the present invention is to easily control the particle size without changing the emulsion composition, and to obtain an emulsion having a narrow particle size distribution, a large particle size, and excellent emulsion stability and compounding stability.

[0004]

The present inventors have conducted intensive studies to achieve the above object. As a result, water having a phase inversion point or higher was added to a mixture of the silicone and the surfactant at a time, and the remaining mixture was stirred. The present inventors have found that an emulsion having a narrow particle size distribution can be obtained by dilution with water, and that the obtained particle size can be controlled by changing the amount of water added first, and the present invention has been completed. That is, in the present invention, in producing an O / W type silicone emulsion of a polyorganosiloxane, water having a phase inversion point or higher is added at once to a mixture of a polyorganosiloxane and a surfactant, followed by mixing and stirring. A method for producing a silicone emulsion, characterized by adding and diluting the remaining water, a silicone emulsion having an emulsion average particle diameter of 1 to 100 μm obtained by the method, and the silicone emulsion. It relates to hair cosmetics.

[0005]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail. Polyorganosiloxane used in the present invention,
Conventionally known ones can be used. For example, _(where R a substituted or unsubstituted monovalent hydrocarbon radical, a is a number of positive than 4) the general formula _{R a SiO (4-a)} / 2 are exemplified those represented by the.
In the formula, R is a substituted or unsubstituted monovalent hydrocarbon group, which may be the same or a plurality of types, for example, an alkyl group such as a methyl group, an ethyl group, a hexyl group, and a decyl group. Group, aryl group such as phenyl group, aralkyl group such as 2-methylphenylethyl group, amino-containing group such as 3-aminopropyl group and 2-aminoethyl-3-aminopropyl group, polyoxyethylene group, polyoxypropylene Groups, polyoxyalkylene groups such as polyoxyethylene-polyoxypropylene groups, and fluorine-containing groups such as 3,3,3-trifluoropropyl groups.
These can be selected according to the purpose and purpose of use. For example, in the case of hair cosmetics, a methyl group is preferable when the purpose is to impart a smooth feeling to hair, and a moist feeling imparting effect and an improvement in adhesion are provided. Various R 1 can be selected, for example, an amino group-containing group is preferable for the purpose, and an aryl group is preferable for the purpose of improving gloss. A is a positive number less than 4, and is preferably from 1.0 to 2.5 from the viewpoint of ease of emulsification and usefulness of the obtained siloxane. One or more polyorganosiloxanes may be used. For example, in addition to giving the hair an excellent feel, polydimethylsiloxane having a cuticle protection effect and a viscosity exceeding 1 million cSt is poor in spreading to the hair by itself, and to compensate for this, for example, several hundred cP Is generally used in combination with the polydimethylsiloxane. Further, instead of polydimethylsiloxane of several hundred cSt, for example, an isoparaffin-based solvent may be used. Of course, also in this case, the manufacturing method of the present invention can be applied. In the production method of the present invention, an emulsion having a small particle size distribution and good stability can be efficiently obtained, and the obtained emulsion composition has a good feel to hair when used in hair cosmetics. The viscosity is from 10,000 to 100,000,000 cSt, especially from 50,000 to 50,000,000 cS, since the application and good cuticle protection effect are performed.
It is preferred to use polydimethylsiloxane of t.

[0006] The surfactant used in the present invention includes:
Any of a nonionic surfactant, an anionic surfactant, and a cationic surfactant may be used. Nonionic surfactants include glyceryl 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, and polyglycerol fatty acid esters. Polyoxyethylene alkyl ethers such as oxyethylene glycerin fatty acid ester, polyoxyethylene sorbitan fatty acid ester and polyoxyethylene fatty acid ester; polyoxyethylene lauryl ether, polyoxyethylene cetyl ether, polyoxyethylene stearyl ether, polyoxyethylene oleyl ether A polyoxyethylene such as polyoxyethylene octyl phenyl ether and polyoxyethylene nonyl phenyl ether; Alkylphenyl ethers; polyoxyethylene-oxypropylene copolymer; and polyether-modified polydimethylsiloxane is illustrated. Examples of the anionic surfactant include sodium alkylbenzene sulfonate such as sodium hexylbenzenesulfonate, sodium octylbenzenesulfonate, sodium decylbenzenesulfonate, sodium dodecylbenzenesulfonate, sodium cetylbenzenesulfonate, and sodium myristylbenzenesulfonate. Sodium alkylnaphthylsulfonate such as sodium butylnaphthylsulfonate; polyoxyethylene alkyl ether such as sodium polyoxyethylene octyl ether sulfate, sodium polyoxyethylene decyl ether sulfate, sodium polyoxyethylene eicosyl ether sulfate; Sulfuric acid ester sodium salt; polyoxyethylene decyl phenyl ether sulfate Polyoxyethylene mono (alkylphenyl) ether sulfate sodium salt such as ether sodium are exemplified. As the cationic surfactant,
Quaternary such as octyltrimethylammonium chloride, dodecyltrimethylammonium chloride, hexadecyltrimethylammonium chloride, tallow trimethylammonium chloride, coconut oil trimethylammonium chloride, octyldimethylbenzylammonium chloride, decyldimethylbenzylammonium chloride, dioctadecyldimethylammonium chloride Ammonium salts are exemplified. These surfactants are usually
Two or more of the same system or different systems can be used in combination. In the production method of the present invention, the particle size distribution is narrow,
An emulsion having good stability can be obtained, and in the obtained emulsion composition, when used in hair cosmetics, a good feeling is imparted to hair, and therefore at least one kind of nonionic surfactant is used. It is preferable to use those containing above, and it is particularly preferable to use only nonionic surfactants. Among the above-mentioned nonionic surfactants, polyoxyethylene sorbitan fatty acid esters, polyoxyethylene fatty acid esters, and polyoxyethylene alkyl ethers are preferably used. The surfactant is used in an amount of 1 to 30 parts by weight based on 100 parts by weight of the polyorganosiloxane.
If the amount is less than 1 part by weight, sufficient emulsification cannot be achieved, while if the amount exceeds 30 parts by weight, the inherent properties of the silicone are sufficiently exhibited because the amount of the surfactant is large. This is because it may not be done. Preferably, 2 parts per 100 parts by weight of polyorganosiloxane
To 20 parts by weight, particularly preferably 5 to 15 parts by weight.

Conventionally, in the case of preparing an O / W emulsion, an oil phase component and a surfactant are usually mixed by heating if necessary, and further mixed while gradually adding water thereto. Can be In this case, an emulsifier such as a colloid mill, a homomixer, and a pressure homogenizer is used as necessary. For example, in the phase inversion emulsification method described above as a conventional technique,
Water is gradually added to the mixture of the oil phase component and the surfactant. First, after passing through a W / O type, a D phase is formed. The D phase is also referred to as a surfactant phase, and is a liquid crystal phase in which oil and water are arranged in a sandwich type by a lamella phase of the surfactant. Here, transparency appears in appearance. Usually, this point is defined as a phase inversion point. In this liquid crystal phase, the oil droplets are in an infinitely finely dispersed state, where more water is added,
An O / D emulsion is formed. At this time, the continuous phase becomes the D phase without affecting the oil phase that is the dispersed phase. Further, water is added to form an O / W emulsion. By doing so, an O / W emulsion in which oil droplets are finely dispersed can be obtained. In this method, water is gradually added, and the inside of the emulsification system is made uniform at each stage, so that O / W having a uniform small particle size is obtained.
To obtain a type emulsion, that is,
The number of times of water injection is 3 or more times, and in practice, usually 5 to 10 times. In this case, in each case, sufficient stirring is required to make the inside of the system uniform, and a long time is required for production. In addition, the D phase is usually a hard gel, and requires high stirring efficiency and large power to make it uniform. As the viscosity of the emulsified material increases, it becomes more difficult to make the inside of the system uniform. In this case, a part where the stirring is insufficiently apt to exist, and as a result, the particle diameter varies. Because of these things, the particle size distribution of the resulting emulsion is likely to change when the device or scale changes,
There is a problem that control is difficult. The amount of water to be the phase inversion point is determined by adding a small amount of water to the mixture of the oil phase component and the surfactant in advance while maintaining the temperature at a constant temperature, and stirring the mixture. It can be measured by a method such as evaluating the highest point as a phase inversion point.

The present invention is characterized in that water having a phase inversion point or higher is added at a time to a mixed system of an oil phase component and a surfactant, and the amount of water injected is equal to or higher than the above-mentioned amount of the D phase. . Since the amount of water in which the D phase is formed changes depending on the oil phase component and the surfactant used, it is difficult to limit, for example, the amount of water injected to the oil phase component. In the present invention, water is first injected with an amount of 1 to 5 times that amount based on the amount of water at the phase inversion point. This is because if the ratio is less than 1, the mixture of the oil phase component, the surfactant and the water cannot be uniformly dispersed even if the dilution water is added, or it takes a long time to disperse the mixture. In addition, when water of 5 times or more is poured for the first time, the mixture of the oil phase component and the surfactant cannot be dispersed in water, or it takes a long time to disperse the mixture. In order to easily disperse and obtain a uniform particle size distribution in both the water injection step and the dilution step, the amount of water is preferably 1.1 to 3 times, particularly preferably 1.5 to 2 times. According to the present invention, the obtained particle diameter becomes small when water is injected at the phase inversion point and then dilution water is added, and when water at or above the phase inversion point is injected at once, the amount becomes large. Accordingly, the particle size obtained gradually increases. That is, it is possible to control the particle size of the emulsion obtained by changing the initial water injection amount. In the present invention, since the water is basically only injected in two divided portions, the manufacturing process can be shortened. In addition, since a hard gel phase is not formed, it is easy to uniformly mix the inside of the system. That is, it is hardly affected by the device and the scale. This method is suitable for batch-type production as well as continuous production, since the number of production steps is small and it is hardly affected by equipment and scale.

In the method for producing an emulsion of the present invention, as described above, polyorganosiloxane may be emulsified by using an isoparaffin-based solvent in combination. When the obtained emulsion is used in, for example, hair cosmetics, for the purpose of diluting the polyorganosiloxane to give wet spreadability, hexane, a paraffinic solvent such as heptane, toluene, an aromatic solvent such as xylene, Various solvents such as isoparaffinic solvents such as isoheptane and isooctane, chlorine solvents such as chloroform, ester solvents, and glycol solvents are exemplified. Further, silica powder for the purpose of defoaming the obtained emulsion, solid powder such as zeolite for the purpose of imparting thixotropy, waxes such as carnauba wax for the purpose of improving gloss, propyl p-hydroxybenzoate, sodium benzoate, Preservatives such as citric acid and salicylic acid, and thickeners such as alginic acid, gum arabic, casein, methylcellulose, hydroxyethylcellulose, cation-modified etherified cellulose, hydroxypropyldene powder, polyvinyl alcohol, polyvinylpyrrolidone, and bentonite can also be used. The production method of the present invention can also be applied when these are used in combination with a polyorganosiloxane.

The emulsion obtained by the production method of the present invention is characterized in that the particle size distribution is monodisperse and narrow,
Another feature is that the emulsion has excellent stability.
Therefore, when used as a material for cosmetics and the like, the obtained cosmetic has usefulness in that it has excellent storage stability. In the production method of the present invention, the average particle diameter is generally 0.1 to 200 μm
Can be efficiently obtained, but those having a relatively large particle size, for example, 1 to 100 μm, particularly 3 to 80 μm, which have been difficult to obtain those having good stability, can be obtained efficiently. There is a feature. The emulsion having such a large particle diameter obtained by the production method of the present invention is characterized not only in that it has excellent stability, but also when it is incorporated into cosmetics and the like, it exhibits the excellent characteristics inherent to silicone.

[0011]

According to the production method of the present invention, a silicone emulsion having a narrow particle size distribution and good stability can be obtained, and particularly a silicone having a large particle size and good stability which has been difficult to produce until now. There is a feature that an emulsion can be obtained. Further, the emulsion has a feature that the particle size of the emulsion can be easily controlled, and the emulsion is hardly affected by the type and scale of the device, and can be carried out in a manufacturing process shorter than a conventional manufacturing method.

[0012]

The present invention will be described in more detail with reference to the following examples. In the examples, “%” means “% by weight”.
Represents The viscosity indicates a value at 25 ° C. Table 1 shows the composition of the emulsion used in the examples. The particle size of the emulsion was measured by the following method. In each emulsion composition, the phase inversion point at 70 ° C. was measured by the method described below. Table 1 shows the obtained inversion point water amount.

[0013]

[Table 1]

Note) Polydimethylsiloxane 1: 200 cSt polydimethylsiloxane Polydimethylsiloxane 2: 100,000 cSt Polydimethylsiloxane Polydimethylsiloxane 3: 20 million cSt Polydimethylsiloxane Amino-containing siloxane: 1000 cSt, nitrogen atom content 0.9% 2-Aminoethyl-3-aminopropyl group-containing polydimethylsiloxane nonionic surfactant 1: polyoxyethylene (23) lauryl ether nonionic surfactant 2: polyoxyethylene (6) lauryl ether nonionic surfactant 3: Polyoxyethylene (55) monostearate Nonionic surfactant 4: Polyoxyethylene (20) sorbitan monostearate Cationic surfactant 1: Cetyl trimethyl ammonium chloride Emulsion particle size measurement Coulter Company Ltd., LS-type, were used (measurement principle laser diffraction / scattering technology). From the obtained results, the average particle diameter, the mode particle diameter, and the average particle diameter / mode particle diameter were confirmed. The spread of the particle size distribution was determined by the ratio of average particle size / mode particle size. That is, it was determined that the closer this ratio was to 1, the monodisperse and narrower the distribution. -Measurement of phase inversion point water amount After the siloxane component and the activator component were stirred while heating at 70 ° C, water was added in an amount of 1% by weight, and the stirring was repeated. At this time, the point where the transparency of the content was the highest was visually determined, and the water injection amount at that time was defined as the phase inversion water amount.

Example 1 Each component was used so that the total amount of the emulsion composition-1 became 100 g. A mixture of 36 g of polydimethylsiloxane 1 and 24 g of polydimethylsiloxane 3 was placed in a 200 cc flask and heated to 70 ° C. After this, heating at 70 ° C. was continued until all the water was added. Here, 1.2 g of the nonionic surfactant 1 and 3.8 g of the nonionic surfactant 3 were added,
The mixture was manually stirred using a metal spatula. When stirring was continued for about 5 minutes while maintaining the heating at 70 ° C., the nonionic surfactant was melted and mixed with the polydimethylsiloxane. Here, 8 g of water was added as the first water injection, and stirring was further continued. Stirring was continued for about 10 minutes to obtain a transparent gel. Next, 27 g of remaining water was added as diluting water, and the mixture was stirred for about 10 minutes while cooling at 70 ° C. was stopped to obtain a milky white emulsion. Table 2 shows the average particle size, mode particle size, and average particle size / mode particle size of this emulsion. Example 2 The same operation as in Example 1 was carried out except that the initial water injection amount was 10 g and the dilution water amount was 25 g. After the initial water injection and stirring, a viscous slightly transparent milky white liquid was obtained, and finally a milky white emulsion was obtained. Table 2 shows the evaluation results such as the particle diameter. Example 3 The same operation as in Example 1 was carried out except that the initial water injection amount was 12 g and the dilution water amount was 23 g. After the initial water injection and stirring, a viscous slightly transparent milky white liquid was obtained, and finally a milky white emulsion was obtained. Table 2 shows the evaluation results such as the particle diameter. Example 4 The operation was carried out in the same manner as in Example 1 except that the initial water injection amount was 15 g and the dilution water amount was 20 g. After the initial water injection and stirring, a viscous milky white liquid was obtained, and finally a milky white emulsion was obtained. Table 2 shows the evaluation results such as the particle diameter. Example 5 The operation was performed in the same manner as in Example 1 except that the initial water injection amount was 18 g and the dilution water amount was 17 g. After the initial water injection and stirring, a viscous milky white liquid was obtained, and finally a milky white emulsion was obtained. Table 2 shows the evaluation results such as the particle diameter. Example 6 The same operation as in Example 1 was performed except that the initial water injection amount was 22 g and the dilution water amount was 13 g. After the initial water injection and stirring, a viscous milky white liquid was obtained, and finally a milky white emulsion was obtained. Table 2 shows the evaluation results such as the particle diameter. Example 7 Each component was used so that the total amount of the emulsion composition-1 became 1500 g. Add 540 of polydimethylsiloxane 1 to Ajihomomixer (manufactured by Tokushu Kika Co., Ltd.) equipped with a 2 liter container.
g and a mixture of 360 g of polydimethylsiloxane 3 were heated to 70 ° C. This heating was continued until dilution water addition.
The stirring was continued with the paddle mixer rotating at 60 rpm. These stirring conditions were continued until the final emulsion was taken out. 18 g of the nonionic surfactant 1 and 48 g of the nonionic surfactant 3 were added thereto, and stirring was continued for about 20 minutes to melt the nonionic surfactant and mix it with polydimethylsiloxane. Here, 225 g of water was added as initial water injection, and stirring was further continued. Stirring was continued for about 20 minutes to obtain a transparent gel. Next, add 300 g of remaining water as diluting water and stir for about 20 minutes to prepare a milky white emulsion,
Evaluation was performed in the same manner as in Example 1. The seventh embodiment is a modification of the fourth embodiment and a scale-up. Example 8 A milky white emulsion was prepared and operated in the same manner as in Example 7, except that the rotation speed of the paddle mixer was changed to 15 rpm.

Comparative Example 1 Each component was used so that the total of the emulsion composition-1 became 100 g. A mixture of 36 g of polydimethylsiloxane 1 and 24 g of polydimethylsiloxane 3 was placed in a 200 cc flask and heated to 70 ° C. After this, heating at 70 ° C. was continued until all the water was added. Here, nonionic surfactant 1
Was added and 3.8 g of the nonionic surfactant 3 were added, and the mixture was manually stirred using a metal spatula. While maintaining the heating at 70 ° C., stirring was continued for about 5 minutes to melt the nonionic surfactant and mix it with polydimethylsiloxane. 2 g of water was added as the first water injection, and stirring was continued for about 10 minutes. 2g of water
The operation of adding and stirring for 10 minutes was repeated twice. Here, what has been a viscous milky white oil has become a transparent gel. Further, the operation of adding 2 g of water and stirring for 10 minutes is repeated eight times, and then 13 g of water as dilution water
The milky white emulsion was prepared by stopping the heating at 70 ° C. and continuing to stir while allowing to cool, and evaluated in the same manner as in Example 1. Comparative Example 2 An emulsion was prepared in the same manner as in Comparative Example 1, except that heating at 70 ° C. was stopped after completion of stirring after the first water injection.
It was evaluated similarly. Comparative Example 3 Each component was used such that the total of the emulsion composition-1 became 1500 g. Add 540 of polydimethylsiloxane 1 to Ajihomomixer (manufactured by Tokushu Kika Co., Ltd.) equipped with a 2 liter container.
g and a mixture of 360 g of polydimethylsiloxane 3 were heated to 70 ° C. This heating was continued until dilution water addition.
The stirring was continued with the paddle mixer rotating at 60 rpm. These stirring conditions were continued until the final emulsion was taken out. Here, 18 g of the nonionic surfactant 1 and 48 g of the nonionic surfactant 3 were added, and stirring was continued for about 20 minutes to melt the nonionic surfactant and mix it with polydimethylsiloxane. Add 30g of water as the first water injection here
Stirring was continued for 20 minutes. The operation of further adding 30 g of water and stirring for 20 minutes was repeated twice. Here, what has been a viscous milky white oil has become a transparent gel. The operation of adding 30 g of water and stirring for 20 minutes was repeated 8 times, then 195 g of water as diluting water was added, and stirring was continued while heating at 70 ° C. was stopped and the mixture was allowed to cool to prepare a milky white emulsion. Evaluation was performed in the same manner as in Example 1. In addition, the comparative example 3 is obtained by changing the apparatus and increasing the scale of the comparative example 1. Comparative Example 4 An emulsion was prepared and operated in the same manner as in Comparative Example 3 except that the rotation speed of the paddle mixer was changed to 15 rpm. Comparative Example 5 The same operation as in Example 1 was carried out except that the initial water injection amount was 4 g and the dilution water amount was 31 g. Although a viscous slightly transparent milky white liquid was obtained after the initial water injection and stirring, the dilution water did not adapt to the stirring after the addition of the dilution water, and a milky white emulsion could not be obtained.

Example 9 Each component was used so that the total amount of the emulsion composition-2 became 100 g. In a 200 cc flask, a mixture of 36 g of polydimethylsiloxane 1, 24 g of polydimethylsiloxane 3 and 6 g of amino group-containing siloxane was heated to 70 ° C. To this, 1.8 g of the nonionic surfactant 1, 1.1 g of the nonionic surfactant 2 and 3.1 g of the nonionic surfactant 3 were added, and the mixture was manually stirred using a metal spatula. About 5
The stirring was continued for minutes, and the nonionic surfactant was melted and mixed with the polydimethylsiloxane. Here, 8 g of water was added as the first water injection, and stirring was further continued. When stirring was continued for about 10 minutes, a transparent gel was obtained. next,
The remaining 20 g of water was added as dilution water and stirred for about 10 minutes to prepare a milky white emulsion, which was evaluated in the same manner as in Example 1. Example 10 The operation was performed in the same manner as in Example 9 except that the initial water injection amount was 20 g and the dilution water amount was 8 g. After the initial water injection and stirring, a viscous milky white liquid was obtained, and finally a milky white emulsion was obtained. Table 2 shows the evaluation results such as the particle diameter. Example 11 Each component was used so that the total amount of the emulsion composition-3 became 100 g. In a 200 cc flask, a mixture of 44 g of polydimethylsiloxane 1 and 30 g of polydimethylsiloxane 3 was added, and 1.5 g of nonionic surfactant 2 and 0.5 g of cationic surfactant 2 were added thereto. And manually stirred. Stirring was continued for about 5 minutes to mix. Here, 6 g of water was added as initial water injection, and stirring was further continued. about
After stirring for 10 minutes, a transparent gel was obtained. Next, 18 g of remaining water was added as diluting water and stirred for about 10 minutes to prepare a milky white emulsion, which was evaluated in the same manner as in Example 1. Example 12 Example 12 except that the initial water injection amount was 15 g and the dilution water amount was 9 g.
The same operation was performed as in 11. After the initial water injection and stirring, a viscous milky white liquid was obtained, and finally a milky white emulsion was obtained. Table 2 shows the evaluation results such as the particle diameter. Example 13 Each component was used so that the total amount of the emulsion composition-4 became 100 g. 60 g of polydimethylsiloxane 2 was placed in a 200 cc flask and heated to 70 ° C. Here, 1.5 g of nonionic surfactant 1 and 2 g of nonionic surfactant 3 were added.
Then, 2.5 g of Nonionic surfactant 4 was added, and the mixture was manually stirred using a metal spatula. Stirring was continued for about 5 minutes to mix. Here, 10 g of water was added as the first water injection, and stirring was further continued. When stirring was continued for about 10 minutes, a transparent gel was obtained. Next, add 24 g of remaining water as dilution water and stir for about 10 minutes to prepare a milky white emulsion,
Evaluation was performed in the same manner as in Example 1. Example 14 Example 14 except that the initial water injection amount was 15 g and the dilution water amount was 19 g.
The same operation as in 13 was performed. After the initial water injection and stirring, a viscous milky white liquid was obtained, and finally a milky white emulsion was obtained. Table 2 shows the evaluation results such as the particle diameter.

[0018]

[Table 2]

In Examples 1 to 6, the amount of water injected at the first time was changed, but the particle size obtained was changed, and the distribution was small. Example 7 had the same composition as Example 4, except that the apparatus and scale were changed, but the particle size distribution obtained was the same. Further, the eighth embodiment is similar to the seventh embodiment.
The rotation speed of stirring was changed while using the same apparatus and scale, but the particle size distribution obtained was also the same. On the other hand, in Comparative Examples 1 and 2, the particle size obtained at the emulsification temperature was changed, but in Comparative Example 1 where the temperature was high, the distribution was wider. In Comparative Example 3, the apparatus and scale were changed with the same composition and the same temperature as Comparative Example 1, but the obtained particle diameter was small. Further, in Comparative Example 4, the rotation speed of stirring was changed while using the same apparatus and scale as Comparative Example 3, but the obtained particle size was large and the distribution was extremely wide. In Examples 9 to 14, even if the surfactant and the polyorganosiloxane were different, the particle size could be changed by changing the initial water injection amount, and the particle size distribution was relatively narrow.

Examples in which the emulsion of the present invention is used in cosmetics will be described below. Example 15 (Hair setting composition) Using the emulsion prepared in Example 1, a hair setting composition having the following composition was prepared and evaluated. Table 3 shows the results
Shown in Composition Silicone emulsion (Example 1) 5.0% Hydroxyethylcellulose 0.2% Ethyl alcohol 10.0% Fragrance 0.2% Deionized water 84.6% ・ Evaluation method <Suppliable> 4g of hair setting composition to 2g of 25cm long hair and distance of 20cm After the application, the hair was evenly arranged with a commercially available comb before drying, and the hair was dried with warm air at 40 ° C. for 60 minutes, and evaluated according to the following evaluation criteria. ○… There is no stiffness when touched by hand, giving a natural feel. △: There is a slight stiffness when touched by hand. ×: Touching by hand is severe and hard. <Smoothness> After uniformly applying 4 g of the hair setting composition to a 2 g hair having a length of 25 cm from a distance of 20 cm, the hair is removed.
It was dried with warm air at 40 ° C. for 60 minutes, and the state of the comb was evaluated using a commercially available comb according to the following evaluation criteria. ○… The comb passes smoothly without snagging. △: Comb can be passed though there is a catch. ×: Comb does not pass. <Set holding power> After 4 g of the hair setting composition was uniformly applied to 2 g of hair having a length of 25 cm from a distance of 20 cm, the hair was wound around a curler having an outer diameter of 1.2 cm, and heated at 40 ° C. for 60 minutes with warm air. Dried. Then, remove the hair from the curler, measure the length (L1) immediately after hanging vertically in an atmosphere at a temperature of 30 ° C. and a relative humidity of 80% and the length (L2) after leaving for 1 hour,
The curl retention was calculated from the following equation. Curl retention (%) = (25−L2) / (25−
L1) × 100 In addition, those with a curl retention of 60% or more passed (marked with “○” in the table), and those with less than 60% failed (in the table,
"X" mark).

Example 16 A hair setting composition was prepared and evaluated in the same manner as in Example 15, except that the emulsion prepared in Example 4 was used. Table 3 shows the results. Example 17 A hair setting composition was prepared and evaluated in the same manner as in Example 15, except that the emulsion prepared in Example 7 was used. Table 3 shows the results. Example 18 A hair setting composition was prepared and evaluated in the same manner as in Example 15, except that the emulsion prepared in Example 9 was used. Table 3 shows the results. Example 19 A hair setting composition was prepared and evaluated in the same manner as in Example 15, except that the emulsion prepared in Example 11 was used. Table 3 shows the results. Comparative Example 6 A hair setting composition was prepared and evaluated in the same manner as in Example 15, except that the emulsion prepared in Comparative Example 1 was used. Table 3 shows the results. Comparative Example 7 A hair setting composition was prepared and evaluated in the same manner as in Example 15, except that the emulsion prepared in Comparative Example 4 was used. Table 3 shows the results.

[0022]

[Table 3]

Example 20, Comparative Example 8 (Shampoo Composition) Using the emulsion prepared in Example 1 or Comparative Example 1, two types of shampoo compositions having the following compositions were prepared.
evaluated. Composition Silicone emulsion (Example 1 or Comparative example 1) 3.0% Polyoxyethylene lauryl ether 15.0% Diethanolamide laurate 5.0% Fragrance 0.2% Deionized water 76.8% Shampoo composition using the emulsion of Example 1 (Example) In the case of (20), good gloss was given to the hair, a refreshing feel was given, and the stability was also good. On the other hand, the shampoo composition using the emulsion of Comparative Example 1 (Comparative Example 8) was able to impart a slightly good feeling, but was insufficient in imparting gloss and stability to hair. .

Claims (3)

[Claims] In producing an O / W type silicone emulsion of a polyorganosiloxane, water having a phase inversion point or higher is added at once to a mixture of a polyorganosiloxane and a surfactant, and the mixture is stirred. A method for producing a silicone emulsion, comprising adding water and diluting the mixture. 2. A silicone emulsion having an emulsion average particle size of 1 to 100 μm, obtained by the production method according to claim 1. 3. A hair cosmetic comprising the silicone emulsion according to claim 2.