CN1761449A - Cosmetic preparation - Google Patents

Abstract

A cosmetic preparation characterized by containing tetrakistrimethylsiloxysilane, which is represented by the following formula (1). The cosmetic preparation is excellent in use feeling and stability. [(CH3)3SiO]4Si (1) .

Description

cosmetic

technical field

The present invention relates to cosmetics, and more specifically, the present invention relates to cosmetics containing tetrakis(trimethylsiloxy)silane, which do not cause dryness and irritation to the skin, have excellent feeling when applied, and are excellent in stability over time .

Background technique

In order to solve the problems of cyclic siloxanes such as octamethylcyclotetrasiloxane commonly used in cosmetics, that is, problems in the cosmetic manufacturing process and dry feeling, the present inventors invented base) silane (hereinafter may be referred to as "M3T") cosmetics (WO01-15685). However, although problems such as dryness have been alleviated, the feeling when used on the skin is not yet perfect. When M3T is made into emulsified or solid cosmetics, there is still room for improvement in terms of cosmetic feel and stability. Therefore, an object of the present invention is to solve these problems and provide a further improved cosmetic.

Contents of the invention

The present invention relates to cosmetics characterized by containing tetrakis(trimethylsiloxy)silane represented by formula (1).

[(CH ₃ ) ₃ SiO] ₄ Si (1)

Cosmetics containing the aforementioned tetrakis(trimethylsiloxy)silane (hereinafter may be referred to as "M4Q") are known (Japanese Patent Laid-Open No. 10-176059, Japanese Patent Laid-Open No. 2000-281796, WO 00/64401, etc. ). However, in these documents, M4Q is one of the low-boiling point siloxanes, which is equivalent to the above-mentioned cyclic siloxanes, or is merely proposed as one of the MQ resins.

These documents do not describe or suggest that M4Q exerts its advantages over the above-mentioned cyclic siloxanes or M3T and applies it to cosmetics. Also, there is no mention in these documents of the possible skin-irritating impurities contained in the industrially prepared M4Q.

The cosmetic of the present invention described above preferably further contains methyltris(trimethylsiloxy)silane represented by formula (2), or a volatile solvent at 1 atm and 25°C.

[(CH ₃ ) ₃ SiO] ₃ SiCH ₃ (2)

Preferably, the above-mentioned volatile solvent is selected from linear dimethylpolysiloxane with 4 or 5 silicon atoms, cyclic dimethylpolysiloxane with 4-6 silicon atoms, and 1 carbon atom. At least one of a -3 monovalent alcohol and a hydrocarbon having 10-16 carbon atoms.

Preferable embodiments of the cosmetics of the present invention include: W/O emulsified cosmetics, cleansers, skin cleansers, cosmetics containing pigments, oily cosmetics, and solid beauty cosmetics. It is preferable that these cosmetics further contain an ultraviolet protection component.

The present invention also relates to cosmetics, characterized in that the cosmetics contain tetrakis (trimethylsiloxy) silane, and the tetrakis (trimethylsiloxy) silane is obtained by a method comprising the following steps (1)-(4) :

(1) Mixing 2-10 moles of hexamethyldisiloxane and 0.01-0.5 moles of acid catalyst into 1 mole of the following tetraalkoxysilane, and setting the temperature at 0°C or above but less than 30°C;

(2) the step of adding 1 mole of tetraalkoxysilane to the system obtained in step (1);

(3) The step of adding 2.5-10.0 moles of water to the system obtained in step (2) while keeping the temperature at 0° C. or above but less than 30° C., and reacting for 30 minutes to 5 hours; and

(4) a step of reacting at a temperature of 30-100° C. for 30 minutes to 5 hours,

Tetraalkoxysilane represented by the following general formula (A) and hexamethyldisiloxane represented by the following chemical formula (B)

Si(OR) ₄ (A)

(R represents a monovalent hydrocarbon group with 1-10 carbon atoms)

(CH ₃ ) ₃ SiOSi(CH ₃ ) ₃ (B) reaction to obtain.

In the cosmetics obtained by the above method, 1,1,1,5,5,5-hexamethyl-3-trimethylsiloxy-3-hydroxytrisiloxane represented by the following formula (3)

The content of [(CH ₃ ) ₃ SiO] ₃ SiOH (3) is about 1% by mass or less of the total mass of the cosmetic.

The best way to practice the invention

The cosmetic of the present invention is characterized in that: containing tetrakis (trimethylsiloxy) silane represented by following chemical formula (1),

[(CH ₃ ) ₃ SiO] ₄ Si (1).

M4Q is chemically inert and has excellent safety. In addition, it does not give the skin the dry feeling peculiar to cyclic siloxanes, and the feeling upon application is excellent.

The boiling point of M4Q at normal pressure is 222°C. It volatilizes more slowly than M3T, which has a boiling point of 190°C under normal pressure. The viscosity at room temperature is about 3.1 mm ² /s. In the present invention, "volatility" means volatility at 25° C. under 1 atmosphere. M4Q can be arbitrarily mixed in the cosmetics within the range of 0.1-90% by mass, preferably adjusted to an appropriate mixing concentration by combining with other ingredients and depending on the dosage form. If the amount of M4Q is less than the above-mentioned lower limit, the advantages of M4Q cannot be exhibited, and if the amount exceeds the above-mentioned upper limit, the oiliness tends to be too high.

By mixing M4Q and M3T, it is possible to make cosmetics that have desired volatility and make the skin feel more refreshed when applied to the skin. The mixing amount ratio of M4Q and M3T can be appropriately adjusted according to the form of cosmetics and the desired volatilization characteristics, and it is preferable to mix them in the range of 5:95-90:10 (mass %). When mixed within this range, not only the desired volatility but also the desired oiliness can be adjusted, and a highly stable cosmetic can be obtained. For example, make-up primer (underground) material can be mixed according to 60:40-40:60.

The total blending amount of M4Q and M3T is preferably in the range of 0.1-90% by mass, more preferably in the range of 0.5-60% by mass relative to the total amount of the cosmetic. As long as it is in this range, users can actually feel the appropriate volatility adjusted by M4Q and M3T.

In addition to M3T, by using various volatile solvents in combination with M4Q, it is possible to adjust the desired volatility while reducing the oiliness of M4Q, and to prepare cosmetics with a refreshing smear feeling. For example, the combination with lower alcohols such as ethanol and isopropanol is preferable, and especially ethanol can produce a refreshing feeling due to the azeotropic effect with M4Q.

On the other hand, it is preferable to mix one or more kinds selected from isododecane, isodecane, isohexadecane, isoparaffin, linear volatile siloxane, and terpenes. In particular, isododecane, isodecane, and isohexadecane have fast volatilization speeds. Combining with M4Q, it can be made into a sustainable volatilization dosage form. If isododecane, isodecane, and isohexadecane clog the skin, they may cause skin irritation. Therefore, it is preferable to improve the formula to reduce clogging. Preferably, the mass ratio of the above-mentioned volatile solvents to M4Q, and the mixture of M4Q and M3T is in the range of 10:90-90:10 as required.

Use commonly used volatile siloxanes with M4Q to control the rate of evaporation or modify the sensory profile. Examples of the above-mentioned commonly used volatile silicones include cyclic dimethylpolysiloxanes with 4-6 silicon atoms in a limited amount that does not cause a dry feeling, and linear dimethyl polysiloxanes with 4 or 5 silicon atoms. Dimethicone. Examples of the above-mentioned cyclic dimethylpolysiloxane include: octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, etc. same solvent.

For example, when an emulsifier is used in combination to prepare an emulsified cosmetic, the above-mentioned M4Q can provide the emulsified cosmetic with high stability over time. There are O/W type and W/O type of emulsified cosmetics, and any of them can be appropriately selected according to the use of cosmetics, the amount of oil to be mixed, and the like. The emulsifier used can be mixed with nonionic siloxane-based surfactants, such as branched chain siloxane type polyglyceryl modified siloxane, branched chain siloxane type polyether modified siloxane, alkyl. One or more of polyether co-modified siloxane, polyether-modified siloxane, cross-linked polyglyceryl-modified siloxane, sugar-modified siloxane, glyceryl-modified siloxane, especially Preferably selected from branched siloxane type polyglyceryl modified siloxane, branched siloxane type polyether modified siloxane, alkyl polyether co-modified siloxane, polyether modified siloxane One or more of alkane, cross-linked polyglyceryl modified siloxane. These components have excellent compatibility with the volatile siloxane of the present invention, and contribute to the formation of a stable emulsion. Among these emulsifiers, those having an HLB value of 6 or less are particularly preferable combinations for preparing W/O type emulsified cosmetics. It can also be used in combination with other emulsifiers so that the overall HLB value of the emulsifier is 6 or less. The emulsifier described above is preferably used in the range of 0.05 to 20% by mass, more preferably 0.1 to 10% by mass relative to the total amount of the cosmetic. The details of these compounds are described, for example, in JP-A-2002-179548, JP-A-2002-179797, JP-A-2002-179798, JP-A-2002-154917, JP-A-7-252122, JP-A Kaiping No. 9-175928, Japanese Patent Publication No. 44-4679, Japanese Patent Application No. 57-14797, Japanese Patent Application No. 55-18424, Japanese Patent Application No. 10-182354, Japanese Patent Application No. 2001-2555, Japanese Patent Application No. JP-A-2000-63233, JP-A-6-145023, JP-A-7-187945, JP-A-5-112424, JP-A-9-71504, etc.

M4Q has excellent solubility, for example, it can dissolve various silicone-based materials commonly used in cosmetics at high concentrations. As the siloxane-based material, it is preferable to combine with siloxane resin, siloxane-modified organic binder, fluorine-modified siloxane resin, polyamide-modified siloxane, acrylated siloxane, alkacrylic acid Co-modified siloxane, siloxane-modified siloxane, urethane-modified siloxane, alkyl-modified siloxane, etc. are used in combination. These siloxane-based materials can be used by dissolving in conventional low-viscosity dimethyl polysiloxane or cyclic siloxane, etc., but M4Q can dissolve these materials at a higher concentration, and as a result, the amount of carried-out components can be reduced, It has the advantage of increasing the freedom of formulation. In cosmetics, these resin components are preferably used in the range of 0.3-20% by mass relative to the total amount of cosmetics. As long as it is within this range, it is possible to obtain a formulation that exhibits the properties of a silicone resin and is excellent in cosmetic durability. When these compounds correspond to siloxane compounds obtained by modifying siloxane chains or siloxane resins through various modifying groups, the details are described in JP-A-61-161211, JP-A-4 -312511, JP-A 2-42008, JP-9-25218, JP-2003-55155, JP-59-20360, JP-9-110633, JP-6- 9332, Japanese Patent Laid-Open No. 10-29921, French Patent No. 2708199, Japanese Patent Laid-Open No. 3-264510, Japanese Patent Laid-Open No. 4-66513, Japanese Patent Laid-Open No. 5-262987, Japanese Patent Laid-Open No. 5-194147, etc. wait.

The excellent solubility of the above M4Q is suitable for dissolving oily dirt. That is, M4Q is suitable for use as a cleanser for removing oily cosmetics and a cleanser for removing sebum stains. In a preferred embodiment of the present invention, the detergent contains M4Q and a nonionic surfactant. M4Q is preferably mixed in the range of 1 to 50% by mass relative to the total amount of the detergent. As long as it is within this range, effective detergency can be exhibited.

Nonionic surfactants can be used as long as they are generally used in cosmetics. In particular, siloxane-based surfactants are preferably used because they have excellent compatibility with M4Q. Examples of siloxane-based surfactants include: for the dimethyl polysiloxane chain, there is at least one selected from polyoxyalkylene groups, alkyl groups with 2-30 carbon atoms that may be partially substituted by atoms such as fluorine, and alcohols. Modified groups such as hydroxyl, phenyl, glyceryl, polyglyceryl, sugar modified groups, oxazoline groups, perfluoropolyether, etc., and have modifications in the form of side groups, terminal groups or block units The latter modified group has polyoxyalkylene groups, glyceryl groups, polyglyceryl groups, sugar modified groups, perfluoropolyether groups, alcoholic hydroxyl groups and other hydrophilic groups as essential constituent units.

For example: polyether modified organopolysiloxane (alias: polyoxyalkylene modified siloxane or polyether modified siloxane), alkyl polyoxyalkylene co-modified siloxane (alias: polyether modified siloxane) Alkyl Co-modified Siloxane), Fluorinated Dimethiconol, Perfluoroalkyl Polyoxyalkylene Co-modified Siloxane, Perfluoroalkoxy Polyoxyalkylene Co-modified Siloxane , Glyceryl-modified siloxane, polyglyceryl-modified siloxane, perfluoroalkyl-polyglyceryl co-modified siloxane, sugar-modified siloxane, etc. Examples of the polyether-modified organopolysiloxane include KF351, KF6011, KF6012, KF6015, KF6017, KF6026, and FPD6131 manufactured by Shin-Etsu Chemical Co., Ltd.

Sorbitan fatty acid esters, glycerin fatty acid esters, polyglycerin fatty acid esters, propylene glycol fatty acid esters, polyethylene glycol fatty acid esters, sucrose fatty acid esters, polyoxyethylene alkyl ethers, polyoxypropylene Alkyl ether, polyoxyethylene alkylphenyl ether, polyoxyethylene fatty acid ester, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene glycerin fatty acid ester, polyoxyethylene Ethylene propylene glycol fatty acid ester, polyoxyethylene castor oil, polyoxyethylene hydrogenated castor oil, polyoxyethylene phytostanol ether, polyoxyethylene phytosterol ether, polyoxyethylene cholestanol ether, polyoxyethylene cholesteryl ether , alkanolamides, sugar ethers, sugar amides and other non-ionic surfactants. The compounding quantity of this nonionic surfactant is preferably 0.1-25 mass % with respect to the total amount of a cleaning agent, Especially preferably, it is 0.5-10 mass %.

When the detergent is mixed with water to make an emulsified type, it is preferably O/W type. In this case, using an HLB value of 10 or more as the above-mentioned nonionic surfactant has an effective detergency, and therefore preferred.

This cleaner is also available without water. In the case of an oil-based cleanser that does not mix with water, a transparent preparation can be obtained by adjusting the refractive index of the oil.

The form of the cleanser is liquid, spray, sheet, mist, mousse, etc., and it is used for the face, around the eyes, hair, and the whole body.

Next, the cleaning agent will be described. Cleansing agents are used to remove dirt and cosmetics from the skin and scalp even in places where there is no washing facility (Japanese Patent Application Laid-Open No. 5-201851). Conventionally, cyclic siloxanes have been used for this purpose. However, as mentioned above, cyclic siloxanes have a problem of causing a dry feeling on the skin called a dry feeling and having a weak ability to dissolve sebum components. On the other hand, M4Q can produce a cleanser that does not feel dry, has high sebum dissolving power, does not cause irritation or trouble to the skin, and has a good feeling of use.

A preferred embodiment of the invention is a skin cleanser comprising M4Q and methylphenylpolysiloxane. As the methylphenylpolysiloxane, those commonly used in cosmetics can be used, and they are preferably liquid at normal temperature and normal pressure. Preferably, the methylphenylpolysiloxane is used in an amount of 0.5 to 25% by mass relative to the total amount of the cleaning agent. As long as it is in this range, the oily feeling will be less after using the cleanser, which can make the feeling better.

The cleaning agent has a boiling point of 225°C or lower under normal pressure, and preferably further contains a solvent that is volatile at 1 atmospheric pressure and 25°C. The volatile solvents include volatile siloxanes such as methyltris(trimethylsiloxy)silane, cyclic siloxane, linear low-molecular siloxane, ethanol, isopropanol, propanol, etc. Other lower alcohols, light liquid paraffins such as isododecane, etc. Among them, methyltris(trimethylsiloxy)silane and ethanol are highly safe and have excellent compatibility with sebum components, so they are preferably mixed. In addition, water can also be mixed, but since sebum or dirt may be reattached to the skin, it is preferable to mix the amount at 10% by mass or less of the total amount of the cleanser, and it is particularly preferable not to contain it. The composition of cleaning agent is as follows: relative to the total amount of cleaning agent, M4Q is 5-70 mass %, methylphenylpolysiloxane is 0.5-25 mass %, and volatile solvent is 25-94.5 mass %, which can improve Wash effect.

The specific uses of the cleaning agent are: cleaning agent, dry (dry) shampoo, and its form is suitable for liquid, spray, and paper sheet.

M4Q has a high dispersing ability for pigments, and is suitable for mixing as a dispersion medium in cosmetics containing pigments. In the past, the use of ester oil or cyclic siloxane was used to pre-prepared pigment dispersion paste by color called color paste method, and the color of the product was adjusted through their combination. The advantage of this method is that toning is easier. However, ester oil may deteriorate due to mechanical energy during dispersion, causing odor, discoloration, and the like. On the other hand, cyclic siloxane is stable against mechanical force, but its dispersion efficiency is poor, and it is difficult to uniformly disperse the pigment. However, the present invention finds that M4Q is stable to mechanical pulverization, has high dispersion efficiency of colored pigments, and is suitable as a dispersion solvent. Therefore, when various coloring pigments are dispersed and mixed into cosmetics, it is found that the obtained cosmetics have high chroma and bright hues.

As the coloring pigment, any pigment can be used as long as it is used in cosmetics. Regardless of its shape (spherical, rod, needle, plate, amorphous, scale, spindle, etc.) or particle size (smoke, particulate, pigment grade, etc.), particle structure (porous, non-porous, etc.) use. Examples of colored pigments include: inorganic red pigments such as iron oxide, iron hydroxide, and iron titanate; inorganic brown pigments such as γ-iron oxide; inorganic yellow pigments such as iron oxide yellow and loess; , carbon black and other inorganic black pigments, manganese violet, cobalt violet and other inorganic purple pigments, chromium hydroxide, chromium oxide, cobalt oxide, cobalt titanate and other inorganic green pigments, Prussian blue, ultramarine blue and other inorganic blue pigments, tar (タ-ル) series pigments made into lakes, natural pigments made into lakes, and synthetic resin powders made by compounding these powders. Specific examples of tar pigments include Red No. 3, Red No. 104, Red No. 106, Red No. 201, Red No. 202, Red No. 204, Red No. 205, Red No. 220, Red No. 226, Red No. 227, Red No. 228, Red No. 230, Red No. 401, Red No. 505, Yellow No. 4, Yellow No. 5, Yellow No. 202, Yellow No. 203, Yellow No. 204, Yellow No. 401, Blue No. 1, Blue No. 2, Blue No. 201 , Blue No. 404, Green No. 3, Green No. 201, Green No. 204, Green No. 205, Orange No. 201, Orange No. 203, Orange No. 204, Orange No. 206, Orange No. 207, etc. Natural pigments are selected from carmine Acid, shellac acid, safflower, brazilianin, crocin and other pigments. Among them, tar pigments, lakes thereof, and natural pigments are preferable.

These colored pigments are, for example, preferably treated with fluorine compounds (preferably perfluoroalkyl phosphate treatment or perfluoroalkylsilane treatment, perfluoropolyether treatment, fluorosiloxane treatment, fluorinated silicone resin treatment), silicone alkane treatment (preferably methylhydrogenpolysiloxane treatment, dimethylpolysiloxane treatment, vapor phase tetramethyltetrahydrocyclotetrasiloxane treatment), silicone resin treatment (preferably trimethylsiloxy Silicic acid treatment), side group treatment (gas-phase siloxane treatment followed by addition of alkyl chains, etc.), silane coupling agent treatment, titanium coupling agent treatment, silane treatment (preferably alkylsilane or alkylsilazane treatment), oil treatment, N-acylated lysine treatment, polyacrylic acid treatment, metal soap treatment (preferably stearic acid or myristate), acrylic resin treatment, metal oxide treatment, agar treatment, deoxyribonucleic acid treatment For surface treatment such as treatment, it is more preferable to use a plurality of the above-mentioned treatments in combination. Among them, the surface treatment with excellent dispersion properties caused by M4Q preferably includes N ^ε -lauroyl-L-lysine treatment, alkyl silane treatment, and side group treatment, and N ^ε -lauroyl with excellent yield and cost performance is particularly preferred. -L-lysine treatment, alkylsilane treatment.

The mixing amount of M4Q in the dispersion is preferably in the range of 20-90% by mass relative to the total mass of the dispersion. In order to improve the dispersibility of the colored pigment, it is preferable to use a surfactant in combination, and it is particularly preferable to use a silicone-based surfactant having a structure similar to M4Q. Examples of siloxane-based surfactants include polyoxyalkylene groups, alkyl groups with 2 to 30 carbon atoms that may be partially substituted, alcoholic hydroxyl groups, and phenyl groups for dimethylsiloxane chains. , glyceryl, polyglyceryl, sugar modified group, oxazoline group, perfluoropolyether and other modified groups, and have modified groups in the form of side groups, terminal groups or block units, wherein The latter modified group has hydrophilic groups such as polyoxyalkylene groups, glyceryl groups, polyglyceryl groups, sugar modified groups, perfluoropolyether groups, and alcoholic hydroxyl groups as essential constituent units. For example: polyether modified organopolysiloxane (alias: polyoxyalkylene modified siloxane or polyether modified siloxane), alkyl polyoxyalkylene co-modified siloxane (alias: polyether modified siloxane) Alkyl Co-modified Siloxane), Fluorinated Dimethiconol, Perfluoroalkyl Polyoxyalkylene Co-modified Siloxane, Perfluoroalkoxy Polyoxyalkylene Co-modified Siloxane , Glyceryl-modified siloxane, polyglyceryl-modified siloxane, perfluoroalkyl-polyglyceryl co-modified siloxane, sugar-modified siloxane, etc. Examples of the polyether-modified organopolysiloxane include KF6012, KF6015, KF6017, KF6026, and FPD6131 manufactured by Shin-Etsu Chemical Co., Ltd. Examples of other dispersants are preferably used sorbitan fatty acid esters, glycerin fatty acid esters, polyglycerin fatty acid esters, propylene glycol fatty acid esters, polyethylene glycol fatty acid esters, sucrose fatty acid esters, polyoxyethylene alkyl ethers , polyoxypropylene alkyl ether, polyoxyethylene alkylphenyl ether, polyoxyethylene fatty acid ester, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene glycerin fatty acid ester, polyoxyethylene propylene glycol fatty acid ester, polyoxyethylene castor oil, polyoxyethylene hydrogenated castor oil, polyoxyethylene phytostanol ether, polyoxyethylene phytosterol ether, polyoxyethylene cholestanol ether, polyoxyethylene Nonionic surfactants such as ethylene cholesteryl ether, alkanolamide, sugar ether, sugar amide, etc. The nonionic surfactant is preferably mixed in an amount of 0.1 to 20% by mass, particularly preferably 0.5 to 15% by mass, based on the mass of the dispersion.

In this dispersion liquid, the above-mentioned components were dispersed using a pulverizer. It is preferable to prepare a dispersion liquid according to the pigment, and then appropriately combine various dispersion liquids to prepare a desired color. Dispersion methods include wet media pulverizers such as bead mills or Microcross (manufactured by Nara Machinery Co., Ltd.), roll mills, jet mills, ultrasonic pulverizers, and high-pressure impact pulverizers such as Alteima Iza-System (manufactured by Suginomasin Co., Ltd.). , disperser, high-speed homogenizer, homogenizer and other methods. Among them, the use of a wet media type pulverizer is preferred because the degree of pulverization is high, a stable dispersion can be obtained, and the yield is excellent. Wet media pulverizers can be vertical or horizontal, continuous or batch. Using these devices, M4Q is mixed with pigments, and optionally dispersants and oils for pulverization. The crushing conditions are related to the capabilities of each device. Make a graph of crushing time, crushing times, and average particle size or color, and set the conditions for the graph to be in a stable state, which is effective for ensuring the stability of the color of each batch.

Examples of cosmetics suitable for M4Q as a pigment dispersion medium include cosmetic products, especially lipsticks, eyeliners, mascara, eyebrow makeup, eye shadows, nail creams, foundations, cover-up cosmetics, チ-ク, hair dyes, etc.

In addition to the above-mentioned various pigments, oily cosmetics can be obtained by mixing oily substances that are solid or paste at 25°C. In the past, oily cosmetics such as lipsticks have been known to mix volatile siloxanes in order to improve the effect of preventing color migration or to improve durability (Japanese Patent Laid-Open Publication No. 8-92036, Japanese Patent Laid-Open Publication No. 3-77162, Japanese Patent Laid-Open Publication No. 10-29915 Bulletin). However, as mentioned above, volatile silicones, especially cyclic silicones, give users a dry feeling when they are applied and after a certain period of time. On the other hand, by using M4Q, not only does not produce a dry feeling, but it is less volatile than the above-mentioned cyclic siloxanes, so it has excellent stability over time, and excellent pigment dispersibility, so it can obtain excellent brightness and gloss. , Oily cosmetics with high chroma.

In a preferred embodiment of the present invention, the oil-based cosmetic contains M4Q, a pigment, and polybutene. M4Q is preferably used in the range of 0.1-60% by mass, more preferably in the range of 1-50% by mass relative to the total amount of the oily cosmetic. As long as it is within this range, advantages such as preparation stability, color migration prevention effect, and enhancement of chroma can be effectively obtained.

The pigment is preferably used in the range of 0.1 to 50% by mass, more preferably in the range of 0.5 to 35% by mass, based on the total amount of the oil-based cosmetic. As long as it is within this range, the stability of the preparation is ensured and there are advantages of excellent feeling.

The polybutene is preferably obtained by copolymerization of isobutene and n-butene, and is more preferably liquid to paste at normal temperature. The polybutene preferably has an average molecular weight of polybutene in the range of 500-2700, more preferably in the range of 800-1200. If the average molecular weight is less than 500, there will be problems with high-temperature stability, and if it is 2700 or more, the sticky feeling will become stronger and the feeling will be bad.

In order to improve stability, the polybutene used in the present invention may be hydrogenated or purified. The blending amount of the polybutene is preferably 2 to 40% by mass relative to the total amount of the oily cosmetic. If it is less than 2% by mass, the sustained-release property of M4Q cannot be controlled, and if it exceeds 40% by mass, the feeling of stickiness will be enhanced and the feeling will be deteriorated.

This oil-based cosmetic can be prepared by a conventionally known method. For example, it can be prepared with a disperser such as a roll or a bead mill, or it can be prepared by mixing the color paste with a bead mill or the like. M4Q is a volatile substance, and the container needs to use a closed container.

This oil-based cosmetic is suitable for lipstick, foundation, eyeshadow, eyeliner, mascara, チ-ク, cover-up cosmetics, sunscreen, makeup primer, etc.

In addition to the above-mentioned pigments and oily substances, by using a surfactant, mixing water, a solid cosmetic cosmetic can be prepared. In the present invention, preferred aspects of cosmetic cosmetics are as follows. Here, each compounding amount is an amount relative to the total mass of cosmetics.

(A) 10-30% by mass of M4Q,

(B) 5-10% by mass of one or more polyol compounds selected from polyvalent alcohols and sugars,

(C) 1.5-3.5% by mass of one or more surfactants selected from sorbitan fatty acid esters, polyglycerol fatty acid esters, sucrose fatty acid esters, and polysaccharide alkyl ethers,

(D) 3-7% by mass of an oily substance that is solid or pasty at 25°C,

(E) 30-45% by mass of pigment, and

(F) 5-25% by mass of purified water.

(B) Examples of polyol compounds include: ethylene glycol, propylene glycol, butylene glycol, diethylene glycol, dipropylene glycol, glycerin, diglycerin, sorbitol, Malbitol, trehalose, raffinose, xylose Alcohol, mannitol, hyaluronic acid or its salt, trehalose derivatives, raffinose derivatives, glycols such as polyethylene glycol and polyglycerin, polysaccharides, and the like. Examples of trehalose derivatives or raffinose derivatives include alkyl ether derivatives or alkenyl ether derivatives of these sugars, particularly preferably alkyl ether derivatives having 1 to 24 carbon atoms and 3 or more carbon atoms. -24 alkenyl ether derivatives. Polysaccharides include: カラギナ-ン, agar, guaiac gum, locust bean gum, gum arabic, tragacanth gum, pectin, xanthan gum, dextran, cellulose, etc. This polyhydric alcohol is mixed in the range of 5-10 mass % with respect to the whole amount of solid beauty cosmetics. If the blending amount of the polyhydric alcohol is less than the above-mentioned lower limit, the skin will feel tight after application, and if it exceeds the above-mentioned upper limit, the skin will feel sticky, which is not preferable.

(C) The above-mentioned various surfactants can be used in the solid cosmetics of the present invention, but among them, from the viewpoint of excellent stability and excellent feeling, it is preferable to use a surfactant selected from sorbitan isostearate, sorbitan at least one monooleate. The blending amount of the surfactant is in the range of 1.5 to 3.5% by mass relative to the total amount of the solid cosmetic cosmetic. If the blending amount is less than the above lower limit, water resistance and sebum resistance may be weakened, and if it exceeds the above upper limit, there may be a problem of stickiness.

(D) Solid or pasty oily substances include not only oily solvents and resins used in conventional cosmetics, but also resins and binders that dissolve in other oily solvents and form a paste at room temperature. Representative examples include: ホホバ wax, carnauba wax, candelilla wax, rice bran wax, shellac, lanolin, beeswax, white wax, ozokerite, ceresin wax, paraffin wax, microcrystalline wax, petrolatum, lauric acid, meat wax, etc. Myristic Acid, Palmitic Acid, Stearic Acid, Behenic Acid, 12-Hydroxystearic Acid, Undecylenic Acid, Lauryl Alcohol, Myristyl Alcohol, Cetyl Alcohol, Stearyl Alcohol, Oleyl Alcohol, Behenyl Alcohol, Squalyl Alcohol Heparyl Alcohol, Chimeryl Alcohol, Squalyl Alcohol, Isostearyl Glyceryl Ether, Ethyl Stearate, Butyl Stearate, Myristyl Myristate, Cetyl Myristate, Stearyl Myristate Cetyl ricinoleate, Cetyl ricinoleate, Glyceryl tri(undecylenate), Pentaerythritol tetramyristate, Cetyl lactate, Octyl hydroxystearate, Cholesteryl stearate, Isostearyl Cholesteryl Hydroxystearate, Cholesteryl Hydroxystearate, Cholesteryl Oleate, Dihydrocholesteryl Oleate, Phytosteryl Isostearate, Polyethylene Glycol, Polyglycerin, Palm Oil, Coconut Oil, Bovine Oil, hydrogenated oil, horse oil, ciabata-, custard oil or polyethylene, polypropylene, polytetrafluoroethylene, acrylic siloxane, acrylic polymer or its salt, acrylic methacrylic acid copolymer or its salt, polyvinylpyrrolidone And other resins. The mixing amount of the solid or pasty oil agent is 3-7% by mass relative to the total mass of the cosmetic. If the blending amount is less than the above lower limit, it will be difficult to obtain water resistance and sebum resistance, and if it exceeds the above upper limit, it will be difficult to remove cosmetics and the feeling will be deteriorated.

(E) The pigment is mixed in an amount of 30 to 45% by mass based on the total amount of the solid cosmetic cosmetic. If the blending amount is less than the above lower limit, the stability of the cosmetic may not be sufficient, so it is preferable to use it in combination with an oily gelling agent to make a cosmetic at or above the above lower limit. On the other hand, if the blending amount exceeds the above-mentioned upper limit, the feeling of cosmetics will be deteriorated, and removal will be difficult.

As long as the pigment is commonly used in cosmetics, any of hydrophilic pigments and hydrophobic pigments can be used, and hydrophobic pigments are particularly preferably used. Commonly used pigments include, for example, inorganic powders, organic powders, surfactant metal salt powders, colored pigments, pearlescent pigments, metal powder pigments, natural pigments, and the like.

In addition to the aforementioned colored pigments, tar pigments, and natural pigments, inorganic powders include pigment-grade titanium oxide, zirconia, pigment-grade zinc oxide, cerium oxide, magnesium oxide, barium sulfate, calcium sulfate, magnesium sulfate, calcium carbonate, Magnesium carbonate, talc, mica, kaolin, sericite, muscovite, synthetic mica, phlogopite, red mica, biotite, lepidolite, silicic acid, silicic anhydride, aluminum silicate, magnesium silicate, aluminum magnesium silicate, silicon Calcium acid, barium silicate, strontium silicate, tungstate metal salt, hydroxyapatite, vermiculite, hidilite, bentonite, montmorillonite, hectorite, zeolite, ceramic powder, calcium hydrogen phosphate, alumina, Aluminum hydroxide, boron nitride, boron nitride, silicon dioxide, titanium oxide particles, low-acidity Chitan particles, zinc oxide particles, cerium oxide particles, activity-inhibited cerium oxide particles, etc.; examples of organic powders include: polyamide powder, polyester powder, polyethylene powder, polypropylene powder, polystyrene powder, polyurethane powder, benzoguanamine powder, polymethylbenzoguanamine powder, polytetrafluoroethylene powder, polymethyl methacrylate powder, fiber Plain, silk powder, nylon powder, 12 nylon, 6 nylon, silicone powder, silicone rubber powder, silicone elastomer spherical powder, polymethylsilsesquioxane spherical powder, polyalkylsilsesquioxane Powder, styrene-acrylic copolymer, divinylbenzene-styrene copolymer, vinyl resin, urea resin, phenol resin, fluororesin, silicone resin, acrylic resin, melamine resin, epoxy resin, polycarbonate resin, Microcrystalline cellulose powder, starch powder, lauroyl resin, etc.; examples of surfactant metal salt powder (metal soap): zinc stearate, aluminum stearate, calcium stearate, magnesium stearate, myristic acid Zinc, magnesium myristate, zinc cetyl phosphate, calcium cetyl phosphate, sodium cetyl zinc phosphate, etc.; examples of pearlescent pigments are: titanium oxide coated mica, titanium oxide coated mica, chlorine oxide Bismuth, titanium oxide coated bismuth oxychloride, titanium oxide coated talc, fish scale foil, titanium oxide coated colored mica, etc. In the same manner as above, various surface treatments can be given to these pigments.

(F) Purified water is mixed in the range of 5-25 mass % with respect to the solid beauty cosmetic total amount. If the mixing amount of purified water is less than the above lower limit, the good feeling will be lost, and if it exceeds the above upper limit, the stability of the formulation may be impaired. As the pure water, ultrapure water, mineral water, hot spring water, etc. may be used.

The obtained solid cosmetic cosmetic has a solid appearance and is made to flow by rubbing, and is filled in an airtight container for use. The specific application of the solid beauty cosmetic of the present invention is not particularly limited, and it is suitable for cosmetic products, especially foundation, concealer cosmetics, eye shadow, lipstick, skin care products, UV protection products, or daily sunscreen preparations.

As mentioned above, we found that M4Q is suitable for the production of various cosmetics with excellent characteristics, but in the production process, 1,1,1,5,5,5-hexamethyl-3-trimethylsilane produced as a by-product Oxy-3-hydroxytrisiloxane (may be referred to as M3Q(OH) hereinafter) causes a big problem in terms of sensation. That is, when 1,1,1,5,5,5-hexamethyl-3-trimethylsiloxy-3-hydroxytrisiloxane is placed on the skin as a liquid, it exhibits an unfavorable strong effect as a cosmetic. Slippery surface. After smearing, the skin will have a rough feeling within about 5 minutes, and after about 10 minutes, it will completely evaporate and return to the original skin feeling, giving people a great change in feeling.

Various studies were carried out for this purpose and it was found that the preferred amount of 1,1,1,5,5,5-hexamethyl-3-trimethylsiloxy-3-hydroxytrisiloxane in cosmetics is 1.0 % by mass or less, more preferably 0.5% by mass or less, further preferably 0.35% by mass or less. It can be seen that in order to make the content of 1,1,1,5,5,5-hexamethyl-3-trimethylsiloxy-3-hydroxytrisiloxane within the above range, it is preferable to make it about 3% by mass in M4Q or less, more preferably about 1.0% by mass or less, further preferably about 0.5% by mass or less. However, the boiling point of 1,1,1,5,5,5-hexamethyl-3-trimethylsiloxy-3-hydroxytrisiloxane is close to that of M4Q. If there is more than 3% by mass, considerable time, energy and cost are required to remove it by distillation purification. Therefore, a method for producing M4Q that minimizes the residue of 1,1,1,5,5,5-hexamethyl-3-trimethylsiloxy-3-hydroxytrisiloxane has been studied. It was found that: by the method containing the following steps (1)-(4):

(1) Mixing 2-10 moles of hexamethyldisiloxane and 0.01-0.5 moles of acid catalyst into 1 mole of the following tetraalkoxysilane, and setting the temperature at 0°C or above but less than 30°C;

(2) the step of adding 1 mole of tetraalkoxysilane to the system obtained in step (1);

(3) keeping the temperature at 0°C or above but less than 30°C, while adding 2.5-10.0 moles of water to the system obtained in step (2), and reacting for 30 minutes to 5 hours; and

(4) a step of reacting at a temperature of 30-100° C. for 30 minutes to 5 hours,

Tetraalkoxysilane represented by the following general formula (A) and hexamethyldisiloxane represented by the following chemical formula (B)

Si(OR) ₄ (A)

(R represents a monovalent hydrocarbon group with 1-10 carbon atoms)

(CH ₃ ) ₃ SiOSi(CH ₃ ) ₃ (B)

The substance prepared by the reaction has a small amount of 1,1,1,5,5,5-hexamethyl-3-trimethylsiloxy-3-hydroxytrisiloxane, which can be achieved without purification such as distillation The above-mentioned about 3% by mass or less is suitable for cosmetics. In the present invention, the purity of M4Q, for example, can be analyzed by gas chromatography and quantified with an area fraction of 100, and the specific method is shown in the examples.

In the formula (A), R is a monovalent hydrocarbon group with 1-10 carbon atoms, examples of which include ethyl, n-propyl, isopropyl, n-butyl, isobutyl, sec-butyl, tert-butyl, n-hexyl group, octyl group, 2-ethylhexyl group, nonyl group, decyl group, and R may be the same or different from each other. Among them, ethyl or isopropyl is particularly preferred.

This tetraalkoxysilane can be used by purifying a substance synthesized by a conventional method, and a reaction solution synthesized from tetrachlorosilane and alcohol by dehydrochlorination reaction can be used without purification. Unpurified tetraalkoxysilane obtained from tetrachlorosilane and alcohol by dehydrochlorination reaction is usually of high purity and contains alcohol and a small amount of disiloxane as impurities. There is no problem if the purity of the unpurified tetraalkoxysilane used in this reaction is 50% or more, preferably 80% or more, particularly preferably 90% or more.

The above preparation method preferably uses 2-10 moles of hexamethyldisiloxane relative to 1 mole of tetraalkoxysilane, more preferably 2.5-5.0 moles. If hexamethyldisiloxane is less than 2.0 moles, the reaction intermediate alkoxy body (1,1,1,5,5,5-hexamethyl-3-trimethylsilyloxy-3-methoxy tri Siloxane ({(CH ₃ ) ₃ SiO} ₃ SiOCH ₃ , hereinafter referred to as M ₃ Q(OMe)) or 1,1,1,5,5,5-hexamethyl-3-trimethylsiloxane The remaining amount of 3-ethoxytrisiloxane ({(CH ₃ ) ₃ SiO} ₃ SiOCH ₂ CH ₃ , hereinafter abbreviated as M3Q(OEt), etc.) increases, so the reaction yield decreases, even if it exceeds 10.0 Mole, there is also the problem that the yield is not expected to increase, and the pot yield (yield per unit total mass of raw materials) decreases.

In the above-mentioned step (1), it is preferable to add 0.5-10.0 moles of monovalent lower alcohols with 1-6 carbon atoms relative to 1 mole of the above-mentioned tetraalkoxysilane, and its specific examples include methanol, ethanol, n-propanol, isopropanol Alcohol, n-butanol, isobutanol, pentanol, hexanol, preferably methanol, ethanol, isopropanol.

The usage-amount of the monovalent lower alcohol used here is 0.5-10 mol with respect to 1.0 mol of tetraalkoxysilanes, Especially preferably, it is 1-5 mol. If the amount of the monovalent lower alcohol is less than 0.5 mol, the dispersibility of water necessary for the hydrolysis reaction will be insufficient, and the residual amount of the reaction intermediate will increase or the yield of high boiling point substances will increase, resulting in a low yield. When it exceeds 10 mol, there exists a problem that a can yield falls.

When using tetramethoxysilane represented by the chemical formula Si(OCH ₃ ) ₄ as tetraalkoxysilane, it is preferable to use 2.0-10.0 moles of hexamethyldisiloxane relative to 1 mole of tetramethoxysilane, 1.0-5.0 moles A monovalent lower alcohol selected from methanol, ethanol, and isopropanol, 0.01-0.5 moles of acid catalyst, 2.5-10.0 moles of water, the step of adding water is reacted at a temperature of 0°C or above but less than 30°C for 30 minutes to 5 hours, After the addition of water is completed, react at a temperature of 30-100°C for 30 minutes to 5 hours to perform a hydrolysis and condensation reaction.

R in tetraalkoxysilane is a silane other than methyl, especially when it is tetraethoxysilane or tetrapropoxysilane, while the hydrolysis reaction is carried out, by-product ethanol or propanol, water and Since the dispersibility of the alkoxysilane becomes better, there is an advantage that it is not necessary to use a monovalent lower alcohol as a solvent. In terms of pot yield, a synthesis method that does not require a monovalent lower alcohol is particularly preferred.

Examples of acid catalysts include sulfuric acid, hydrochloric acid, methanesulfonic acid, trifluoromethanesulfonic acid and the like. Sulfuric acid and trifluoromethanesulfonic acid are particularly preferably used. The amount of the acid catalyst used is preferably 0.01-0.5 mol, more preferably 0.02-0.4 mol, based on 1 mol of tetraalkoxysilane. If the amount of the acid catalyst is less than 0.01 mol, the reaction rate becomes slow and the reaction time becomes longer, and if it exceeds 0.5 mol, the yield of high-boiling point substances increases, resulting in a problem that the yield decreases.

Water used in this reaction may be used alone or water to which a monovalent lower alcohol having 1 to 6 carbon atoms has been added. When a monovalent lower alcohol is added to water, the alcohol may be methanol, ethanol, n-propanol, isopropanol, n-butanol, isobutanol, or the like. The total amount of monovalent lower alcohols used is preferably within the molar ratio range described above.

The amount of water used in this reaction is preferably 2.5-10.0 mol, more preferably 3.0-8.0 mol, based on 1 mol of tetraalkoxysilane. If the trialkoxysilane is less than 2.5 moles, the residual amount of the alkoxy body (M3Q(OMe), M3Q(OEt), etc.) as a reaction intermediate increases and the yield decreases, but even if it exceeds 10 moles, the yield is hopeless Raise, the problem that tank yield reduces occurs.

In this reaction, it is preferable to first mix hexamethyldisiloxane and a monovalent lower alcohol having 1 to 6 carbon atoms as required, and then mix the acid catalyst and tetraalkoxysilanes. Hexamethyldisiloxane, alcohol, acid catalyst, tetraalkoxysilane can also be mixed simultaneously, but preferably the temperature of the reaction mixture is 0°C or above but less than 30°C, preferably 0°C or More than but less than 25°C, particularly preferably 0°C to 15°C. Add water under the state that temperature is lower than above-mentioned lower limit value, then reaction velocity becomes slow, thereby reaction time is too long; And add water under the state that temperature exceeds above-mentioned upper limit value, then the yield of target substance, M4Q reduces, Therefore, it is not preferable.

In order to further increase the yield of M4Q, hexamethyldisiloxane and, if necessary, a monovalent lower alcohol can be mixed so that the temperature of the mixture is 0°C or more but less than 30°C. Preference is given to 0-25°C, particularly preferably 0-15°C. The acid catalyst is added thereto while the above temperature does not exceed 30°C, preferably does not exceed 25°C, particularly preferably does not exceed 15°C, and is stirred at this temperature for 10 minutes to 1 hour. Next, tetraalkoxysilane is preferably added at a rate such that the temperature of the reaction mixture is kept at 0° C. or above but less than 30° C., preferably at a rate of 0-25° C., particularly preferably at a rate of 0-15° C. Stir at this temperature for 10 minutes to 1 hour, then add water.

In this reaction, water is further added to carry out hydrolysis, but adding water is exothermic, so it is preferable to add while cooling to keep the temperature of the reaction mixture at 0°C or more but less than 30°C. When water is added, if the internal temperature is lower than 0°C, the reaction rate will be slow and the reaction time will be too long; and if the internal temperature is 30°C or above, the yield of the target product will decrease. It is preferably added while maintaining a temperature of 0-25°C, and particularly preferably added while maintaining a temperature of 0-15°C. After the addition of water is completed, it is further preferable to continue stirring at 0°C or more but less than 30°C for 10 minutes to 5 hours.

After the above steps, in the reaction, it is preferable to further heat the temperature of the reaction mixture to 30-100° C., preferably 40-80° C., and keep stirring for 30 minutes to 5 hours, preferably 1 hour to 3 hours. In this way, the residual amount of alkoxy bodies (M3Q(OMe), M3Q(OEt), etc.) and M3Q(OH), which are reaction intermediates, is reduced, and the yield of the target M4Q is increased.

In this method, it is preferable to separate the aqueous layer by liquid separation after the reaction, and to neutralize the organic layer with an aqueous alkali solution such as sodium bicarbonate. Then wash the organic layer until the washing solution is neutral, and carry out distillation and purification, or add anhydrous sodium sulfate or calcium chloride and other desiccants to the reaction solution after washing for dehydration, and then carry out distillation and purification.

Hereinafter, for reference, a conventional synthesis method will be described. The synthesis method for obtaining M4Q may refer to the synthesis method of methyltris(trimethylsiloxy)silane (M3T). Known methods for preparing M3T currently include the following methods.

1. A method of cohydrolyzing methyltrichlorosilane and trimethylchlorosilane in the presence of methanol (International Publication No. WO 2001-15658, Japanese Patent Laid-Open No. 2002-68930).

2. A method of reacting methyltrichlorosilane with hexamethyldisiloxane in the presence of a perchloric acid catalyst (Dokl. Akad. Nauk SSSR, 227, 607-610 (1976)).

3. A method of reacting methyltriethoxysilane with hexamethyldisiloxane in the presence of an acidic ion exchange resin (J. Organomet. Chem., 340, 31-36 (1988)).

4. A method of reacting methyltrialkoxysilane and hexamethyldisiloxane in the presence of a carboxylic acid and an acid catalyst (Japanese Patent Laid-Open No. 11-217389).

5. A method in which concentrated sulfuric acid is added to methyltrimethoxysilane, hexamethyldisiloxane and methanol, and then a mixture of water and methanol is added dropwise to react (International Publication No. WO 2001-15658, Japanese Patent Laid-Open 2002- Bulletin No. 68930).

The method of 1 needs a large amount of water, and the selectivity of reaction is low, so yield is very low.

The method of 2 requires the use of perchloric acid which is difficult to obtain as a catalyst, and is not suitable as an industrial production method.

In the method of 3, in order to increase the reaction rate, it is necessary to use a large excess of hexamethyldisiloxane. In the synthesis of methyltris(trimethylsiloxy)silane, there are 1,1,1,3,5,5,5-heptamethyl-3-ethoxytrisiloxane as a reaction intermediate ({(CH ₃ ) ₃ SiO} ₂ Si(OCH ₂ CH ₃ )CH ₃ , hereinafter abbreviated as M2T(OEt)) remains in large quantities. Also, when a trimethylsiloxy group is introduced into a silicon atom, three trimethylsiloxy groups are introduced when synthesizing methyltris(trimethylsiloxy)silane, but the reactivity of the third one is higher than that of the second one. low. When synthesizing tetrakis(trimethylsiloxy)silane, four trimethylsiloxy groups are introduced, so it is expected that the reactivity of the fourth trimethylsiloxy group is higher than that of methyl tri(trimethylsiloxy group). ) The reactivity of the third trimethylsiloxy group in the silane synthesis is further reduced. Therefore, when considering the synthesis of tetrakis (trimethylsiloxy) silane in the same way, the residual amount of M3Q (OEt) as a reaction intermediate is more, and it is not suitable as a method for obtaining high-purity tetrakis (trimethylsiloxy) silane. Silane method.

In method 4, the reaction intermediate M2T(OEt) remains in the synthesis of methyltris(trimethylsiloxy)silane. Therefore, when tetrakis(trimethylsiloxy)silane is synthesized in the same way, it is expected to be used as a reaction intermediate The residual amount of M3Q (OEt) of the body is more, and it cannot be satisfied as an effective method for obtaining high-purity tetrakis (trimethylsiloxy) silane.

In method 5, similar to the above, the reaction intermediate {(CH ₃ ) ₃ SiO} ₂ Si(CH ₃ )OCH ₃ (hereinafter referred to as M2T) remains in the synthesis of methyltris(trimethylsiloxy)silane. (OMe)), so when synthesizing tetrakis (trimethylsiloxy) silane in the same way, it is expected that the residual amount of M3Q (OMe) as a reaction intermediate is more, which cannot meet the requirement of effectively obtaining high-purity tetrakis (trimethylsiloxy) silane. siloxy) silane method.

As shown in Tables 1 and 2 of Examples described later, compared to the above-mentioned conventional methods, according to the method of the present invention, a product having an M3Q(OH) amount of about 3% by mass or less before purification can be obtained.

The impurities in the prepared M4Q can be analyzed by gas chromatography, and the analysis conditions are as follows.

Shimadzu Gas Chromatograph GC14B

Column packing trade name SE30, liquid phase 3% grade

Column inner diameter 5mm, length 3m

Detector TCD, injection temperature 80°C

Furnace temperature 80°C, holding time 1 minute, heating rate 15°C/min, final temperature 300°C

When analyzed under the above conditions, M3Q (OMe) was detected at 6.2 minutes, M3Q (OEt) at 6.3 minutes, M3Q (OH) at 6.6 minutes, M4Q at 7.5 minutes, and high boiling point components were detected between 10.5 and 13.0 minutes. .

An example of the finally obtained physical property data of M4Q is shown below.

Appearance: colorless transparent liquid

Boiling point: 215°C (1 atmosphere), 89.5-90.0°C/1.3kPa

Viscosity: (25°C); 3.1mm ² /s

Specific gravity: (25°C); 0.864

Refractive index: (25°C); 1.387

Freezing point: -70°C or below

The M4Q is preferably mixed in various cosmetics mentioned above. In the range that does not impair the purpose of the present invention, the cosmetics of the present invention can use various components commonly used in cosmetics, such as UV protection components, oil agents, preservatives, fragrances, moisturizers, thickeners, in addition to the above-mentioned components. , salts, solvents, antioxidants, chelating agents, neutralizing agents, pH regulators, insect repellents, physiologically active ingredients and other ingredients.

Inorganic and organic substances can be used as the UV protection component. Examples of inorganic UV protection components include metal oxides such as titanium dioxide, subacidized Chitan, zinc oxide, cerium oxide, and active-sealed cerium oxide, metal hydroxides such as iron hydroxide, plate-shaped iron oxide, aluminum flakes, etc. Metal flakes, silicon carbide and other ceramics. Among them, at least one selected from metal oxide fine particles or metal hydroxide fine particles having an average particle diameter in the range of 5 to 100 nm is particularly preferable. As with the above-mentioned pigments, various surface treatments can also be applied.

Examples of organic UV protection ingredients include 2-ethylhexyl p-methoxycinnamate (alias: octyl p-methoxycinnamate), 2-hydroxy-4-methoxybenzophenone, 2-hydroxy- 4-methoxybenzophenone-5-sulfuric acid, 2,2'-dihydroxy-4-methoxybenzophenone, p-methoxyhydrocinnamic acid diethanolamine salt, p-aminobenzoic acid (hereinafter referred to as PABA), PABA ethyl dihydroxypropyl ester, PABA glyceride, homomenthyl salicylate, methyl anthranilate, 2-ethylhexyl-2-cyano-3,3-diphenylacrylic acid Esters, octyldimethyl PABA ester, octyl salicylate, 2-phenyl-benzimidazole-5-sulfuric acid, triethanolamine salicylate, 3-(4-methylbenzylidene) camphor, 2, 4-dihydroxybenzophenone, 2,2',4,4'-tetrahydroxybenzophenone, 2,2'-dihydroxy-4,4'-dimethoxybenzophenone, 2- Hydroxy-4-N-octyloxybenzophenone, 4-isopropyldibenzoylmethane, 4-tert-butyl-4'-methoxydibenzoylmethane, octyltriazone, 4 -(3,4-dimethoxyphenylmethylene)-2,5-dioxo-1-imidazolidinylpropionate 2-ethylhexyl ester, its polymer derivatives, and silane derivatives, etc. .

It is also possible to use a polymer powder in which an organic UV protection component is encapsulated. The polymer powder can be hollow or not, the average primary particle size can be in the range of 0.1-50 μm, and the particle size distribution can be broad or narrow. The types of polymers include acrylic resins, methacrylic resins, styrene resins, polyurethane resins, polyethylene, polypropylene, polyethylene terephthalate, silicone resins, nylon, acrylamide resins, and the like. Among these polymer powders, powders in which an organic UV protection component is encapsulated within a range of 0.1 to 30% by mass of the powder are preferred, and it is particularly preferred to mix the UVA absorber 4-tert-butyl-4'-methoxydibenzoylmethane .

Among the above-mentioned anti-ultraviolet components, from the viewpoint of common use, easy acquisition, and high anti-ultraviolet effect, it is preferably selected from titanium oxide particles, zinc oxide particles, 2-ethylhexyl p-methoxycinnamate, 4-tert-butyl - at least one of 4'-methoxydibenzoylmethane and benzophenone-based ultraviolet absorbers. It is particularly preferable to use an inorganic system and an organic system in combination. It is also preferred to use a combination of UV-A-corresponding and UV-B-corresponding.

Examples of commonly used oil agents used in the present invention are: avocado oil, linseed oil, almond oil, ibodo wax, perilla oil, olive oil, cocoa butter, kapok wax, torreya oil, carnauba wax, liver oil, Candelilla Wax, Shea Butter, Beef Hoof Oil, Beef Bone Oil, Hardened Beef Butter, Almond Oil, Spergiwax, Hardened Oil, Wheat Germ Oil, Sesame Oil, Rice Germ Oil, Rice Bran Oil, Sugarcane Wax, Camellia Oil, Saffron Oil , ciabata-, tung oil, cinnamon oil, jojoba wax, shellac wax, turtle oil, soybean oil, tea seed oil, camellia oil, evening primrose oil, corn oil, lard oil, rapeseed oil, Japanese tung oil, bran wax , germ oil, horse oil, パシツク oil, palm oil, palm kernel oil, castor oil, hardened castor oil, castor oil fatty acid methyl ester, sunflower oil, grape oil, bay seed wax, hohoba oil, macadamia nut oil, beeswax , Mink Oil, Cottonseed Oil, Cotton Wax, Tree Wax, Tree Wax Nuclear Oil, Montan Wax, Coconut Oil, Hydrogenated Coconut Oil, Triple Coco Fatty Acid Glycerides, Suet, Peanut Oil, Lanolin, Liquid Lanolin, Reduced Lanolin , lanolin alcohol, hard lanolin, lanolin acetate, lanolin fatty acid isopropyl ester, hexyl laurate, POE lanolin alcohol ether, POE lanolin alcohol acetate, lanolin fatty acid polyethylene glycol ester, POE hydrogenation Lanolin alcohol ether, egg oil, etc.; examples of hydrocarbon oils are: ozokerite, squalane, squalene, ceresin, paraffin, paraffin, liquid paraffin, pristane, polyisobutylene, microcrystalline wax, petrolatum, etc. ; Examples of higher fatty acids are: lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, undecylenic acid, oleic acid, linoleic acid, linolenic acid, arachidonic acid, eicosapenta Acrylic acid (EPA), docosahexaenoic acid (DHA), isostearic acid, 12-hydroxystearic acid, etc.; examples of higher alcohol-based oils include: lauryl alcohol, myristyl alcohol, palmityl alcohol, stearic acid Fatty Alcohol, Behenyl Alcohol, Cetyl Alcohol, Oleyl Alcohol, Isostearyl Alcohol, Hexyldodecanol, Octyldodecanol, Cetostearyl Alcohol, 2-Decyltetradecyl Alcohol, Cholesterol, Vegetable Sterols, POE cholesteryl ethers, monostearyl glyceryl ethers (batyl alcohol), monooleyl glyceryl ethers (squalyl alcohols), etc.; examples of ester oils are: diisobutyl adipate, adipate 2-Hexyldecyl Isostearate, Di-2-Heptyl Undecyl Adipate, N-Alkyl Glycol Monoisostearate, Isocetyl Isostearate, Triisostearyl Trimethylolpropane fatty acid, ethylene glycol di-2-ethylhexanoate, hexadecyl 2-ethylhexanoate, trimethylolpropane tri-2-ethylhexanoate, tetramethylhexanoate -Pentaerythritol 2-ethylhexanoate, cetyl caprylate, octyldodecylgum ester, oleyl oleate, octyldodecyl oleate, decyl oleate, isononanoic acid Isononyl Ester, Neopentyl Glycol Dicaprate, Triethyl Citrate, 2-Ethylhexyl Succinate, Amyl Acetate, Ethyl Acetate, Butyl Acetate, Isohexadecyl Stearate Esters, Butyl Stearate, Diisopropyl Sebacate, Di-2-Ethylhexyl Sebacate, Cetyl Lactate, Myristyl Lactate, Isopropyl Palmitate, 2-Palmitate Ethylhexyl ester, 2-hexyldecyl palmitate, 2-heptylundecyl palmitate, cholesteryl 12-hydroxystearate, dipentaerythritol fatty acid ester, isopropyl myristate, myristate Octyldodecyl myristate, 2-hexyldecyl myristate, myristyl myristate, hexyldecyl dimethyl octanoate, ethyl laurate, hexyl laurate, N-lauroyl- L-glutamic acid-2-octyldodecyl ester, diisostearyl malate, etc.; examples of glyceride oils are: acetylglyceryl, glyceryl triisocaprylate, glyceryl triisostearate , Glyceryl Triisopalmitate, Glyceryl Tri(Capryl Caprate), Glyceryl Monostearate, Glyceryl Di-2-heptylundecanoate, Glyceryl Trimyristate, Isomyristate Diglyceryl stearate, etc.

Dimethylorganopolysiloxane, amino-modified organopolysiloxane, alcoholic hydroxyl group-containing organopolysiloxane, alkyl-modified organopolysiloxane other than methyl group or phenyl group, amojimechon, etc. Silicone oil has excellent compatibility with M4Q and can be used preferably. The siloxane chain length of these silicone oils is not limited, and can be used as long as the degree of polymerization is in the range of about 1 to 30,000.

Fluorocarbons such as fluorine-modified siloxane, perfluoropolyether, fluorinated pitch, perfluorodecalin, perfluorooctane, etc., fluoroalcohols, perfluoroalkyl alkyl ethers and other fluorine-based oils can also be mixed , to obtain a formulation with properties. In particular, fluorine-modified siloxane, perfluoroalkylbiphenyl-modified siloxane, or perfluoropolyether are preferred because of their versatility.

Examples of humectants include sugar alcohols such as sorbitol, maltose, and maltol; sterols such as cholesterol, sitosterol, phytosterol, and lanosterol; glucose, sucrose, lactose, raffinose, trehalose, xylitol, and glycerin , propylene glycol, dipropylene glycol, tripropylene glycol, polypropylene glycol, 1,3-butanediol, ethylene glycol, diethylene glycol, triethylene glycol, diglycerin, polyglycerin, hyaluronic acid and its salts, sulfuric acid Chondroitin and its salts, pyrrolidone carboxylate, polyoxyethylene methyl glucoside, polyoxypropylene methyl glucoside, ethyl glucoside, etc.

Examples of thickening agents are: gum arabic, tragacanth, arabinogalactan, locust bean gum (carob), guaiac gum, karaya gum, karage-nan, pectin, agar, quince seeds ( Quince), starch (rice, corn, potato, wheat), algecoroid, trrant gum, locust bean gum and other plant-based polymers, xanthan gum, dextran, succinyl glucan, pullan and other microbial-based polymers, Collagen, casein, albumin, gelatin and other animal-based polymers, carboxymethyl starch, methyl hydroxypropyl starch and other starch-based polymers, methyl cellulose, ethyl cellulose, methyl hydroxypropyl cellulose, Carboxymethylcellulose, hydroxymethylcellulose, hydroxypropylcellulose, nitrocellulose, sodium cellulose sulfate, sodium carboxymethylcellulose, crystalline cellulose, cellulosic polymer of cellulose powder, seaweed Alginic acid-based polymers such as sodium phosphate and propylene glycol alginate, vinyl-based polymers such as polyvinyl methyl ether, polyvinylpyrrolidone, and carboxyvinyl polymers, polyoxyethylene-based polymers such as polyethylene glycol, Oxyethylene polyoxypropylene copolymer polymers, acrylic polymers such as sodium polyacrylate, polyethyl acrylate, and polyacrylamide, polyethyleneimine, cationic polymers, bentonite, magnesium aluminum silicate, raponet, smectite, Inorganic thickeners such as saponite, hectorite, silicic anhydride, etc. Other thickeners include oil-soluble gelling agents, such as metal soaps selected from aluminum stearate, magnesium stearate, zinc myristate, N-lauroyl-L-glutamic acid, α, γ- Amino acid derivatives such as di-n-butylamine, dextrin fatty acid esters such as dextrin palmitate, dextrin stearate, dextrin 2-ethylhexanoic acid palmitate, sucrose palmitate, sucrose stearate Benzylidene derivatives of sorbitol such as sucrose fatty acid esters, monobenzylidene sorbitol, dibenzylidene sorbitol, dimethyl benzyl dodecyl ammonium montmorillonite clay, dimethyl dioctadecyl At least one gelling agent of organically modified clay minerals such as alkylammonium montmorillonite and octadecyldimethylbenzylammonium montmorillonite.

As the surfactant, in addition to the nonionic ones described above, anionic or cationic surfactants can be appropriately used depending on the type of preparation. Examples of anionic surfactants include fatty acid soaps such as sodium stearate and triethanolamine palmitate, alkyl ether carboxylic acids and their salts, carboxylates such as condensation of amino acids and fatty acids, alkylsulfonic acids, and alkenesulfonic acids Salts, sulfonates of fatty acid esters, sulfonates of fatty amides, sulfonates of alkyl sulfonates and their formaldehyde condensates, alkyl sulfates, higher secondary alcohol sulfates, alkyl and allyl Ether sulfates, sulfates of fatty acid esters, sulfates of fatty acid alkylolamides, sulfates of Turkish red oil, etc., alkyl phosphates, ether phosphates, alkyl allyl ether phosphates Salt, amide phosphate, N-acyl amino acid active agent, etc.; examples of cationic surfactants include: alkyl amine salt, polyamine and amino alcohol fatty acid derivatives and other amine salts, alkyl quaternary ammonium salt, aromatic quaternary Ammonium salts, pyridinium salts, imidazolium salts, etc.

Examples of preservatives are: alkyl parabens, benzoic acid, sodium benzoate, sorbic acid, potassium sorbate, phenoxyethanol, etc.; examples of antibacterial agents are: benzoic acid, salicylic acid, carbolic acid, sorbic acid , Alkyl p-hydroxybenzoate, p-chloro-m-cresol, hexachlorophenol, chlorbenzylamine, chlorhexidine chloride, trichloro-carbanilide, triclosan, photosensitizer, phenoxyethanol wait.

Physiologically active ingredients can be substances that impart some physiological activity to the skin when applied to the skin. Such as anti-inflammatory agent, anti-aging agent, UV protection agent, tightening agent, antioxidant, hair growth agent, hair growth agent, moisturizing agent, blood circulation promoter, antibacterial agent, sterilizer, desiccant, cooling agent, warming agent , Vitamins, Amino Acids, Healing Accelerators, Stimulus Relief Agents, Analgesics, Cell Activators, Enzyme Ingredients, etc. Among them, natural plant extract components, seaweed extract components, and crude drug components are particularly preferable. In the present invention, it is preferable to mix one or more of these physiologically active ingredients.

Examples of these physiologically active ingredients include: Ashitaba (Ashitaba) extract, Avocado (Abogado) extract, Amachiya (Amacha) extract, Marshmallow (Altea) extract, Arnica flower (Arunika) extract, aloe (アロエ) extract, apricot extract, almond extract, ginkgo extract, fennel extract, turmeric (ウコン) extract, oolong tea extract, rose hip (エイジツ) extract, echinacea (Echinashi) leaf extract , Scutellaria baicalensis extract, Phellodendron phellodendri extract, Coptis chinensis extract, Barley extract, Hypericum (Otogiri sow) extract, Wild sesame (Odrico sow) extract, Water celery (Orandakalashi) extract, Orange extract, Dried sea water , seaweed extract, hydrolyzed elastin, hydrolyzed wheat flour, hydrolyzed silk, chamomile (カモミラ) extract, carrot (カロツト) extract, capillary wormwood (カワラヨヨヨギ) extract, licorice extract, hibiscus flower (カルカデ) extract extract, firethorn (カキヨク) extract, kiwi fruit (キウイ) extract, cinchona (キナ) extract, cucumber (キュ-カンバ-) extract, guanosine, gardenia (クチナシ) extract, bamboo (クマザサ) extract, locust tree (クララ) extract, walnut (クルミ) extract, grapefruit extract, クレマテイイス extract, chlorella (クロレラ) extract, mulberry extract, gentian (Genchina) extract, Black tea extract, yeast extract, burdock (Gobo) extract, rice bran fermented extract, rice germ oil, daisy (Confri-) extract, collagen, bilberry (Kokemomo) extract, Asarum (Syshin) extract, Bupleurum (サイコ) extract, umbilical cord (サイタイ) extract, sage (Salvia) extract, soapwort (Subonso) extract, bamboo (Sasa) extract, hawthorn (Sanzashi) extract, Zanthoxylum bungeanum (Sanshiヨウ) Extract, shiitake (Shiitake) extract, Rehmannia glutinosa (Giou) extract, purple root (Sikon) extract, perilla (Siso) extract, linden (Sinanoki) extract, Spiraea (Simotsukesow) extract, peony (シヤクヤク) extract, calamus (シヨウブ) root extract, white birch (シラカバ) extract, horsetail (スギナ) extract, foreign ivy extract, hawthorn (セイヨウスンザシ) extract, Western elderberry (セィヨウニワトコ) extract yarrow (セイヨウノコギリソウ) extract, peppermint (セイヨウハツカ) extract, sage (セ-ジ) extract, mallow (ゼニアオイ) extract, Chuanxiong (センキユウ) extract, Swertia (センブリ) extract, soybean (ダイズ) extract, jujube (タイソウ) extract, thyme (タイム) extract, tea extract, clove (ヨヨジ) extract, Imperata (Chigaya) extract, tangerine peel (Chimpi) extract Angelica (Touki) Extract, Toukinsenka Extract, Peach Kernel Extract, Spruce (Touhe) Extract, Hodgami (Dokudami) Extract, Tomato Extract, Natto Extract, Ginseng Extract, Garlic Extract , wild rose (Nobara) extract, hibiscus (Hibiscus) extract, Ophiopogon japonicus (Bakumondo) extract, lotus (Hasu) extract, parsley (Paseri) extract, honey, witch hazel (Hamamelis) extract , Wallweed (Parietaria) Extract, Japan Tongquan Grass (Hikiokoshi) Extract, Bisabolol, Loquat Extract, Coltsfoot (Fukitanpopo) Extract, Butterbur Leaf (Fukinoto) Extract, Poria (Bukuriyo) Extract , ブツチヤ-ブル-ム extract, grape extract, propolis, loofah (ヘチマ) extract, safflower (ベニバナ) extract, mint leaf (pepa-mint) extract, Nanjing linden (Bodaiju) extract, peony ( Botan) extract, hops (hops) extract, pine (matsu) extract, horse chestnut (maronie) extract, Guanyin lotus (mizubashiyo) extract, sapinberry (mukuroji) extract, melissa (melissa) Extract, peach extract, cornflower (Yagulmagik) extract, eucalyptus (ユ-カリ) extract, saxifrage (ユキノシタ) extract, yuzu (ユズ) extract, coix seed (ヨクイニン) extract, mugwort Artemisia (ヨモギ) extract, lavender (ラベンダ-) extract, apple extract, lettuce (レタス) extract, lemon extract, milk vetch (レンゲソウ) extract, rose extract, rosemary (ロ-ズマリ-) extract, white chamomile extract, royal jelly (ロ-ヤルゼリ-) extract, etc.

There are also biopolymers such as deoxyribonucleic acid, mucopolysaccharides, sodium hyaluronate, sodium chondroitin sulfate, collagen, elastin, chitin, chitosan, hydrolyzed egg shell membrane, glycine, valine , Leucine, Isoleucine, Serine, Threonine, Phenylalanine, Arginine, Lysine, Aspartic Acid, Glutamic Acid, Cystine, Cysteine, Methionine amino acids such as acid and tryptophan, hormones such as estradiol and vinyl estradiol, amino acids, sodium lactate, urea, sodium pyrrolidone carboxylate, betaine, whey and other moisturizing ingredients, sphingosine, ceramide, cholesterol, Cholesterol derivatives, phospholipids and other oily ingredients; ε-aminocaproic acid, glycyrrhizic acid, β-glycyrrhetinate, lysozyme chloride, guaiazulene, hydrocortisone, allantoin, tranexamic acid, azulene, etc. Anti-inflammatory agents; vitamins A, B2, B6, C, D, E, calcium pantothenate, biotin, niacinamide, vitamin C esters and other vitamins, allantoin, diisopropylamine dichloroacetate, 4-aminomethyl Cyclohexane carboxylic acid and other active ingredients, tocopherol, carotenoid, flavonoid, tannin, xylan, saponin, butyl hydroxyanisole, dibutyl hydroxytoluene, phytic acid, etc. Antioxidant, α-hydroxy acid, β-hydroxy acid and other cell stimulators, γ-oryzanol, vitamin E derivatives and other blood circulation promoters, retinol and retinol derivatives and other healing agents, Tetrandrine , licorice extract, capsicum tincture, hinoki alcohol, iodized garlic extract, pyridoxine hydrochloride, d1-α-tocopherol, acetic acid d1-α-tocopherol, niacin, niacin derivatives, calcium pantothenate, D - Panthenol, Panthenyl Ethyl Ether, Biotin, Allantoin, Isopropylmethylphenol, Estradiol, Ethinyl Estradiol, Capronium Chloride, Benadryl Chloride, Diphenhydramine Hydrochloride, Takana Cooling agents such as -lu, camphor, salicylic acid, vanilla nonanoic acid amide, vanilla nonanoic acid vanilla amide, pirocton olamine, glyceryl pentadecanoate, 1-menthol, camphor; mononitroguaiac wood Phenol, resorcinol, γ-aminobutyric acid, γ-amino-β-hydroxybutyric acid, benzethonium chloride, slow heart rhythm hydrochloride, plant growth hormone, estrogen, cantharidin tincture, cyclosporine, pyridoxine Zinc sulfide, hydrocortisone, stalactin, polyoxyethylene sorbitan monostearate, peppermint oil, sasanishiki extract and other hair growth agents, etc.

Examples of pH regulators include lactic acid, citric acid, glycolic acid, succinic acid, tartaric acid, d1-malic acid, potassium carbonate, sodium bicarbonate, ammonium bicarbonate, etc. Examples of chelating agents include: alanine, sodium edetate Salt, sodium polyphosphate, sodium metaphosphate, phosphoric acid, etc.

Examples of solvents include water such as purified water, mineral water, and deep ocean water, as well as light liquid isoparaffins, ethers, LPG, N-methylpyrrolidone, next-generation prolon, and the like.

In addition to the above, cosmetics containing M4Q may be skin care products, hair products, antiperspirant products, beauty products, UV protection products, fragrance products, and the like. For example, there are lotions, creams, lotions, calamine lotions, sunscreens, makeup primers, tanning agents, after-shave lotions, pre-shave lotions, facial masks, cleansers, facial cleansers, and anti-acne Basic cosmetics such as cosmetics and essence, beauty cosmetics such as foundation, white powder, eye shadow, eyeliner, eyebrow cream, チ-ク, nail cream, lipstick, lipstick, etc., shampoo, conditioner, conditioner, hair dye, hair toner, Styling agent, talcum powder, hair nourishing agent, deodorant, depilatory agent, soap, bath liquid, bath agent, hand soap, perfume, etc. The form of the product is not particularly limited, and may be liquid, emulsion, cream, solid, paste, gel, powder, multilayer, mousse, spray, etc.

Example

The present invention will be described in detail below using Examples and Comparative Examples, but the present invention is not limited thereto. Unless otherwise specified, the unit of the following mixing amount is mass %.

Preparation Example (Preparation of Tetrakis(trimethylsiloxy)silane)

According to the addition ratios in Table 1 and Table 2, the hydrolysis reaction was carried out according to the following steps 1-6 to obtain tetrakis(trimethylsiloxy)silane.

Tetrakis(trimethylsiloxy)silane was prepared by the following procedure.

(Step 1) Install a reflux condenser, a thermometer and a stirrer on a 1000ml four-necked glass flask, and replace the inside with nitrogen. Hexamethyldisiloxane and alcohol were added to the flask, and the flask was cooled in an ice-water bath so that the internal temperature was 10°C.

(Step 2) Keeping the internal temperature at 10°C, the acid catalyst was added dropwise thereto over 30 minutes, and stirred at 10°C for 30 minutes as it was.

(Procedure 3) Next, keeping the internal temperature at 10° C., alkoxysilane was added dropwise thereto over 45 minutes, and stirred at that temperature for 1 hour as it was.

(Step 4) Keep the internal temperature at 10°C, add water dropwise over 1 hour, and then stir at 5-25°C for 1 hour after the dropwise addition.

(Step 5) Heat to make the internal temperature 50° C., and stir for 2 hours.

(Step 6) The resulting reaction solution was separated, the aqueous layer was separated, and the organic layer was washed with sodium bicarbonate and then with water. (the result that gained organic layer is carried out gas chromatographic analysis is shown in table 1, table 2.)

[Gas Chromatography Analysis Conditions]

Device used: Shimadzu GC14B

Column filler: trade name SE 30 (3% liquid phase, column inner diameter 5mm, length 3m)

Detector: TCD

Column injection temperature: 80°C, the retention time at 80°C is 1 minute, the heating rate is 15°C/min, and the final temperature is 300°C

The resulting organic layer was distilled, and the fraction with a boiling point of 89.5-90.0° C./1.3 kPa was taken out to obtain tetrakis(trimethylsiloxy)silane with a purity of 99.5% or above.

[distillation conditions]

The distillation apparatus used McMahon packing, and used a distillation column with an inner diameter of 2.5 cm and a length of 70 cm. Identification of impurities and target substances was performed by mass spectrometry and NMR analysis.

Table 1 Add substance Preparation Example 1 Preparation Example 2 Preparation Example 3 Preparation Example 4 step 1 Hexamethyldisiloxane 486.0g (3.0 moles) 648.0g (4.0 moles) 486.0g (3.0 moles) 486.0g (3.0 moles) alcohol Methanol 96.0g (3.0 moles) Methanol 96.0g (3.0 moles) none Ethanol 46.0g (1.0 mole) step 2 acid catalyst Concentrated sulfuric acid 9.8g (0.1 mole) Concentrated sulfuric acid 9.8g (0.1 mole) Concentrated sulfuric acid 9.8g (0.1 mole) Trifluoromethanesulfonic acid 7.5g (0.05mol) step 3 Tetramethoxysilane 152.0g (1.0 mole) 152.0g (1.0 mole) - - Tetraethoxysilane - - 208.0g (1.0 mole) 208.0g (1.0 mole) step 4 water 90.0g (5.0 moles) 90.0g (5.0 moles) 90.0g (5.0 moles) 72.0g (4.0 moles) analysis results Halfway organic layer analysis (GC analysis result) (area%) M3Q(OMe) 5.2 1.8 - - M3Q(OEt) - - 4.5 6.7 M3Q(OH) 1.1 0.3 0.9 1.8 Tetrakis(trimethylsiloxy)silane 91.7 97.2 93.4 89.6 high boiling point substances 2.0 0.7 1.2 1.9 Distillation result Yield (g) 332.2 361.0 344.1 316.0 Yield (%) 86.5 94.0 89.6 82.3 Tank yield (%) 39.8 36.3 41.0 40.9 GC analysis result (area %) of final purification M3Q(OMe) less than 0.1 less than 0.1 - - M3Q(OEt) - - less than 0.1 less than 0.1 M3Q(OH) less than 0.1 0.3 0.2 less than 0.1 Tetrakis(trimethylsiloxy)silane 99.9 or above 99.7 99.8 99.9 or above high boiling point substances less than 0.1 less than 0.1 less than 0.1 less than 0.1

Table 2 Add substance Preparation Example 5 Preparation Example 6 step 1 Hexamethyldisiloxane 405.0g (2.5 moles) 486.0g (3.0 moles) alcohol Methanol 96.0g (3.0 moles) Ethanol 46.0g (1.0 mole) step 2 acid catalyst Concentrated sulfuric acid 19.6g (0.2 mole) Concentrated sulfuric acid 9.8g (0.1 mole) step 3 Tetramethoxysilane 152.0g (1.0 mole) - Tetraethoxysilane - 152.0g (1.0 mole) step 4 water 90.0g (5.0 moles) 144.0g (8.0 moles) analysis results Halfway organic layer analysis (GC analysis result) (area%) M3Q(OMe) 8.7 - M3Q(OEt) - 4.4 M3Q(OH) 3.1 0.6 Tetrakis(trimethylsiloxy)silane 84.2 94.1 high boiling point substances 4.0 0.9 Distillation result Yield (g) 309.1 346.4 Yield (%) 80.5 90.2 Tank yield (%) 40.5 41.3 GC analysis result (area %) of final purification M3Q(OMe) less than 0.1 - M3Q(OEt) - less than 0.1 M3Q(OH) less than 0.1 0.2 Tetrakis(trimethylsiloxy)silane 99.9 or above 99.8 high boiling point substances less than 0.1 less than 0.1

In the table, M3Q(OMe) is {(CH ₃ ) ₃ SiO} ₃ SiOCH ₃ , M3Q(OEt) is {(CH ₃ ) ₃ SiO} ₃ SiOCH ₂ CH ₃ , M3Q(OH) is {(CH ₃ ) ₃ SiO} ₃ SiOH, that is, 1,1,1,5,5,5-hexamethyl-3-trimethylsiloxy-3-hydroxytrisiloxane. The yield was determined from the molar ratio of the target tetrakis(trimethylsiloxy)silane and the tetraalkoxysilane used for the reaction.

Prepare Comparative Example

According to the addition ratio shown in Table 3, the hydrolysis reaction was carried out according to the above steps 1-6, the distillation conditions were changed, and more fractions containing M3Q(OH) were recovered, and fine-tuned with purified tetrakis(trimethylsiloxy)silane, A solution containing 35% M3Q(OH), 65% tetrakis(trimethylsiloxy)silane was obtained. The GC analysis results of the solution are shown in Table 4.

table 3 Add substance Prepare Comparative Example step 1 Hexamethyldisiloxane 486.0g (3.0 moles) alcohol Ethanol 46.0g (1.0 mole) step 2 acid catalyst Concentrated sulfuric acid 9.8g (0.1 mole) step 3 Tetramethoxysilane - Tetraethoxysilane 152.0g (1.0 mole) step 4 water 36.0g (2.0 moles) analysis results Halfway organic layer analysis (GC analysis result) (area%) M3Q(OMe) - M3Q(OEt) 0.7 M3Q(OH) 18.2 M4Q 65.8 high boiling point substances 15.3

Table 4 GC analysis results (area%) M3Q(OMe) - M3Q(OEt) M3Q(OH) 35 M4Q 65 high boiling point substances 0.1

Examples and comparative examples of the cosmetics of the present invention are given below. Tetrakis(trimethylsiloxy)silane (M4Q) used below is the compound prepared in Preparation Example 1. As methyltris(trimethylsiloxy)silane (M3T), TMF-1.5 manufactured by Shin-Etsu Chemical Co., Ltd. was used.

Example 1 (Cleansing Gel)

Prepare the cleansing gel according to the recipe and preparation method described below.

formula

(1) Ethanol 3.0

(2) Glycerin 5.0

(3) Dimethicone (Note 1) 8.0

(4)Tetrakis(trimethylsiloxy)silane 15.0

(5) Polyether modified polysiloxane (Note 2) 7.0

(6) P.O.E (60 moles) hydrogenated castor oil 1.0

(7) Octyldodecyl myristate 2.0

(8) Vitamin E (acetate) 0.1

(9) Oleyl alcohol 0.3

(10) Alkyl modified carboxy vinyl polymer 0.5

(11)Carboxyvinyl polymer 0.2

(12) Methylparaben 0.3

(13) Potassium hydroxide hair 0.4

(14) Phenoxyethanol 0.2

(15) Purified water up to 100

Note 1: Sirin KF-96-100cs (manufactured by Shin-Etsu Chemical Co., Ltd.)

Note 2: Silicon KF-351 (manufactured by Shin-Etsu Chemical Co., Ltd.)

Preparation:

Mix and dissolve the oil components (1)-(9) evenly. Then (10)-(15) are uniformly mixed and dispersed, and the previously mixed and dissolved oil components are added. Mix and disperse with a homogenizer, then fill into a tube to obtain a product.

Example 2 (Cleansing Gel)

According to the following recipe, cleansing gel was prepared in the same manner as in Example 1.

formula

(1) Ethanol 3.0

(2) Glycerin 5.0

(3) Dimethicone (Note 1) 5.0

(4)Tetrakis(trimethylsiloxy)silane 10.0

(5) Methyltris(trimethylsiloxy)silane (M3T) 8.0

(6) Polyether modified polysiloxane (Note 2) 7.0

(7) P.O.E (60 moles) hydrogenated castor oil 1.0

(8) Octyldodecyl myristate 2.0

(9) Vitamin E (acetate) 0.1

(10) Oleyl alcohol 0.3

(11) Alkyl modified carboxy vinyl polymer 0.5

(12)Carboxyvinyl polymer 0.2

(13) Methylparaben 0.3

(14) Potassium hydroxide 0.4

(15) Phenoxyethanol 0.2

(16) Purified water up to 100

Note 1: Silicon KF-96-100cs (manufactured by Shin-Etsu Chemical Co., Ltd.)

Note 2: Silicon KF-351 (manufactured by Shin-Etsu Chemical Co., Ltd.)

Comparative example 1

Using volatile cyclic 5-mer siloxane instead of tetrakis(trimethylsiloxy)silane, Example 1 was repeated completely.

Comparative example 2

Example 1 was completely repeated using Silicone KF-96-100cs (manufactured by Shin-Etsu Chemical Co., Ltd.) instead of polyether-modified polysiloxane and P.O.E (60 mol) hydrogenated castor oil.

The sensory properties of each of the above-mentioned cleaning agents were evaluated in accordance with the following evaluation criteria.

[Evaluation criteria for sensory properties]

For each evaluation item, 20 professional evaluators are invited (the evaluators are sometimes repeated for different items), and in each evaluation item, according to the number of evaluators judged to be excellent, the evaluation is performed according to the following categories. All subsequent sensory evaluations used the following evaluation criteria. The number of people who answered "good" out of 20 people evaluate 15 or more people 10-14 people 5-9 people 0-4 people ◎○△×

The evaluation results are shown in the table below.

(sensory properties) Feeling dry after use easy to remove makeup Excellent usability Example 1 Example 2 Comparative Example 1 Comparative Example 2 ◎◎△◎ ◎◎◎× ◎◎◎×

The results in the above table show that compared with the comparative examples, the examples of the present invention are easy to remove makeup, and do not feel dry, and have excellent use feeling.

Embodiment 3 (dry shampoo)

Dry shampoo was prepared according to the following formula and preparation method.

Recipe (Dry Shampoo)

(1)Tetrakis(trimethylsiloxy)silane 47

(2) Methyltris(trimethylsiloxy)silane The balance

(3) Ethanol 12

(4) Methylphenyl polysiloxane 8

(KF56 made by Shin-Etsu Chemical Co., Ltd.)

(5) Isononyl Isononanoate 2

(6) Menthol 0.1

(7) Spices Appropriate amount

(8) Hibiscus extract 0.2

(9) Aloe Vera Extract 0.1

Preparation:

The ingredients are uniformly dissolved and filled into containers.

Comparative example 3

The tetrakis(trimethylsiloxy)silane and methyltris(trimethylsiloxy)silane in Example 3 were replaced with 5-mer cyclic siloxane, and the rest were prepared in the same manner as in Example 3.

Embodiment 4 (paper sheet cleaning agent)

According to the following formula and preparation method, the paper sheet cleaning agent is obtained.

Recipe (paper flake cleaner)

(1)Tetrakis(trimethylsiloxy)silane The balance

(2) Ethanol 20

(3) Methylphenyl polysiloxane 4

(KF56 made by Shin-Etsu Chemical Co., Ltd.)

(4) 1,3-Butanediol 10

(5) Menthol 0.1

(6) Appropriate amount of spices

Preparation:

Dissolve each component evenly, then inject the solution into the non-woven fabric with a dispenser, and seal it with a bag.

Embodiment 5 (paper sheet cleaning agent)

According to the following formulation, it carried out similarly to Example 4, and obtained the paper sheet-shaped cleaning agent.

Recipe (paper flake cleaner)

(1)Tetrakis(trimethylsiloxy)silane The balance

(2) Methyltris(trimethylsiloxy)silane (M3T) 25

(3) Ethanol 15

(4) Methylphenyl polysiloxane 4

(KF56 made by Shin-Etsu Chemical Co., Ltd.)

(5) 1,3-Butanediol 10

(6) Menthol 0.1

(7) Spices Appropriate amount

Comparative example 4

Cyclic tetramer volatile siloxane was used instead of tetrakis(trimethylsiloxy)silane in Example 4, and everything else was prepared in the same manner as in Example 4.

According to the above functional property evaluation classification, each cleaning agent was evaluated, and the results are shown in the table below.

(sensory properties) No dry feeling after use easy to remove dirt Excellent usability Embodiment 3 Comparative Example 3 Embodiment 4 Embodiment 5 Comparative Example 4 ◎×◎◎× ○△◎◎△ ○△◎◎△

The results in the above table show that, compared with the comparative examples, the examples of the present invention are easy to decontaminate, do not feel dry, and have excellent use feeling.

The formulations of the spices used in Examples 3-5 are shown in the table below. spice recipe Element quality‰ Element quality‰ Terpineol 10.00 Vanillin 2.00 Terpine acetate 2.00 Ethyl vanillin 0.10 Sepione-to 60.00 Muscone 0.50 Methyl dihydrojasmonate 250.00 Ethylene tridecanedioate 42.00 indole 0.05 4,6,6,7,8,8-Hexamethyl-1,3,4,6,7,8-Hexahydrocyclopentabenzopyran 60.00 2-Methyl-3-(3,4-methylenedioxy-phenyl)-propanal 3.00 Cyclopentadecanolide 20.00 Hydroxycitronellal 20.00 Ambrette Lactone 1.00 Hydroxycitronellol 10.00 γ-Undecanolide 0.40 p-tert-butyl-α-methylhydrocinnamaldehyde 35.00 γ-Decanolactone 0.10 4-(4-Hydroxy-4-methyl-pentyl)-3-cyclohexene-1-calvokisialde 75.00 4-(4-Hydroxyphenyl)-2-butanone 0.50 3-Methyl-5-phenylpentanol 20.00 Muscone 0.10 Phenyl alcohol 10.00 Skatole 0.01 α-ionone 10.00 cis-jasmone 0.05 β-ionone 20.00 Phenyl ethyl acetate 0.10 γ-Methylionone 10.00 civetone 0.20 Dihydro-β-ionone 25.00 γ-nonanoic acid lactone 0.05 Benzyl salicylate 150.00 α-Santalol 0.20 cis-3-hexenyl salicylate 30.00 β-Santalol 0.20 Eugenol 0.80 Eugenyl acetate 0.10 cinnamyl alcohol 5.00 α-Hexylcinnamaldehyde 20.00 Cinnamic aldehyde 0.50 α-Turkone 0.04 Guaiacyl acetate 1.00 β-Turkone 0.02 Guaiacol 0.50 β-Damascenone 0.01 Cedryl acetate 5.00 δ-Turkone 0.01 cedryl methyl ketone 30.00 rose absolute 0.50 6,7-Dihydro-1,1,2,3,3-pentamethyl-4(5H)-indan 2.00 rose oil 4.50 Vebisyl Acetate 10.00 sandalwood oil 2.00 3-Methyl-5-(2,3,3-trimethyl-3-cyclopenten-1-yl)-pentan-2-ol 2.00 Cistus Absolute Oil 0.05 2-Ethyl-4-(2,3,3-trimethyl-3-cyclopenten-1-yl)-2-buten-1-ol 0.80 sisto absolute 0.01 Isobornylcyclohexanol 35.00 Vetiver Oil 0.50 piperonal 10.00 guaiac wood oil 0.10 Coumarin 2.00 total 1000.00

Embodiment 6 (lipstick)

Lipsticks were prepared according to the formula and preparation method described below. A pigment treated with 8% by mass of ^Nε -lauroyl-L-lysine was used as a coloring pigment, and a pigment treated with 10% by mass of the same substance was used for mica titanium. Titanium oxide treated with 8% by mass of octylsilane was used.

(Preparation of Colored Pigment Dispersion Liquid)

70 parts by mass of tetrakis(trimethylsiloxy)silane was mixed with 30 parts by mass of Surface Treatment Red No. 201. Then, it was ground twice with a sand mill to prepare a dispersion liquid A.

70 parts by mass of tetrakis(trimethylsiloxy)silane was mixed with 30 parts by mass of Surface Treatment Red No. 202. Then, it was ground twice with a sand mill to prepare a dispersion B.

formula

(ingredient A)

(1) Dispersion A 3

(2) Dispersion B 8

(3)Tetrakis(trimethylsiloxy)silane 30

(ingredient B)

(4) Pure ceresine wax 18

(5) castor oil balance

(6) Polybutene 8

(7) Alkyl modified siloxane 1

(ingredient C)

(8) Treatment of titanium oxide 1

(ingredient D)

(8) Processing Mica Titanium 14

Preparation

Mix and dissolve component B, then mix component A, disperse component C into it and knead, finally add component D, disperse evenly, degas it, then pour it into a mold, cool and solidify to obtain a product.

Comparative Example 5

Example 6 was otherwise completely repeated using cyclopentasiloxane (decamethylcyclopentasiloxane) instead of tetrakis(trimethylsiloxy)silane.

Comparative example 6

Dispersion A and Dispersion B used in Example 8 were not pulverized with a sand mill, but only stirred. Using this solution, the preparation method was changed to the following, and Example 6 was completely repeated.

Preparation

Component B was mixed and dissolved, then component C was mixed and dispersed, kneaded, and then component A, component D were added and dispersed. It is degassed, then poured into a mold, cooled and solidified to obtain a product.

The following table shows the sensory property evaluation results of Example 6 of the present invention and Comparative Examples 5 and 6.

(sensory properties) bright colors Have a sense of transparency Smooth application Difficult to fade Example 6 Comparative Example 5 Comparative Example 6 ◎△× ◎△× ◎○× ○○×

The comparison of the examples and comparative examples in the above table shows that the examples of the present invention are bright in color, have a sense of transparency, smooth application, and are difficult to fade. On the other hand, Comparative Example 5 is an example of using a cyclic siloxane conventionally used as a dispersant. Even under the same preparation conditions, the degree of dispersion is low and the color tone of the product is different. Comparative Example 6 is an example in which dispersion is not performed, and has the quality when used as a lipstick conventionally.

Embodiment 7 (lipstick)

Lipsticks were prepared according to the formula and preparation method described below.

A pigment treated with 5% by mass of N ^ε -lauroyl-L-lysine was used.

formula

(ingredient A)

(1)Tetrakis(trimethylsiloxy)silane 40

(2) Trimethylsiloxysilicic acid 2

(ingredient B)

(3) Pure ceresine wax 18

(4) castor oil balance

(5) Polybutene 8

(ingredient C)

(6) Handle red number 202 1

(7) Treatment of titanium oxide 1

(8) Processing Mica Titanium 15

Preparation

Mix and dissolve component B, then disperse and knead component C, then add previously dissolved component A, disperse evenly, degas it, then pour it into a mold, cool and solidify to obtain a lipstick.

Example 8

According to the following recipe, lipstick was prepared in the same manner as in Example 7.

(1)Tetrakis(trimethylsiloxy)silane 20

(2) Methyltris(trimethylsiloxy)silane (M3T) 20

(3) Trimethylsiloxysilicic acid 3

(4) Pure ceresine wax 8

(5) Castor oil 17

(6) Polybutene 10

(7) Methylphenyl polysiloxane 5

(FZ-209: Manufactured by Japan Yunika-Co., Ltd.)

(8) Red No. 202 1

(9) Titanium oxide 1

(10)Mica Titanium 15

Comparative Example 7

Example 7 was otherwise completely repeated using a cyclic pentameric volatile siloxane (decamethylcyclopentasiloxane) instead of tetrakis(trimethylsiloxy)silane.

Comparative Example 8

Use pure ceresine instead of polybutene, other complete repeat embodiment 7.

Comparative Example 9

Using dimethylpolysiloxane (KF96A, 100cs, manufactured by Shin-Etsu Chemical Co., Ltd.) instead of tetrakis(trimethylsiloxy)silane, Example 7 was completely repeated.

The sensory property evaluation results of Examples 7, 8 and Comparative Examples 7-9 are shown in the table below.

(sensory properties) Excellent resistance to color shift over time Shiny bright colors no dryness Smooth application Good spreadability Example 7 ◎ ◎ ◎ ◎ ◎ ◎ Example 8 ◎ ◎ ◎ ◎ ◎ ◎ Comparative Example 7 ○ △ △ x ○ ○ Comparative Example 8 x x x x x x Comparative Example 9 x ○ △ △ x △

The results in the above table show that: compared with the comparative examples, the examples of the present invention have excellent performance in each item. Comparative Example 7 is an example in which conventionally used cyclic siloxane was used instead of tetrakis(trimethylsiloxy)silane, and it was found that a feeling of dryness was felt, and the degree of vividness of the color was also different. In Comparative Example 8, pure ceresin was used instead of polybutene, and the evaluation was poor. In Comparative Example 9, a nonvolatile siloxane was used instead of a volatile substance, and the overall evaluation deteriorated.

Example 9

Obtain solid powder foundation according to following formula and preparation method. A pigment treated with 5% by mass of N ^ε -lauroyl-L-lysine was used.

formula

[Pigment component] (38.2% by mass)

(1) Treatment of spherical titanium oxide (average primary particle size 0.4μm) 18

(2) Treatment of iron oxide (a mixture of iron oxide black, iron oxide red, and iron oxide yellow) 1.7

(3) Treatment of talc 6

(4) Handling mica 2

(5) N ^ε -lauroyl-L-lysine 3.5

(6) Polyalkylmethylsilsesquioxane 5

(average primary particle size 4μm)

(7) Octyl silylated titanium oxide particles 2

(average primary particle size 10nm)

[Liquid Components]

Volatile siloxane (25% by mass)

(8)Tetrakis(trimethylsiloxy)silane 25

Polyol (6.5% by mass)

(9) 1,3-Butanediol 5

(10) Maltol 1

(11)Raffinose 0.5

Surfactant (2% by mass)

(12) Sorbitan Isostearate 2

Solid or pasty oil (5% by mass)

(13) Paraffin 5

Purified water (12.7% by mass)

(14) Purified water 12.7

Oil agent

(15) Dimethicone (6 cs) 3

(16) Methylphenyl polysiloxane 2

(17) Octyl p-methoxycinnamate 2

(18) Propylene glycol dicaprylate 2

(19) Dipentaerythritol hexahydroxystearate 0.5

Physiologically active ingredients

(20) Cranberry (クランベリ-) Extract 1

preservative

(21) Parabens 0.1

Preparation

The oily liquid components were uniformly mixed and dissolved at 80°C. Add premixed and pulverized pigment components thereto, and disperse uniformly at 80°C. An aqueous liquid component previously uniformly mixed and dissolved at 80° C. was added thereto for emulsification and dispersion. Next, the obtained emulsion was degassed, filled into a metal container, and placed in an airtight container to obtain a solid foundation.

Example 10

A solid foundation was obtained in the same manner as in Example 9 according to the following formulation.

formula

[Pigment component] (38.2% by mass)

(1) Treatment of spherical titanium oxide (average primary particle size 0.4μm) 18

(2) Treatment of iron oxide (a mixture of iron oxide black, iron oxide red, and iron oxide yellow) 1.7

(3) Handling of talc 6

(4) Processing mica 2

(5) N ^ε -lauroyl-L-lysine 3.5

(6) Polyalkylmethylsilsesquioxane 5

(average primary particle size 4μm)

(7) Octyl silylated titanium oxide particles 2

(average primary particle size 10nm)

[Liquid Components]

Volatile siloxane (25% by mass)

(8)Tetrakis(trimethylsiloxy)silane 15

(9)Methyltris(trimethylsiloxy)silane 10

Polyol (6.5% by mass)

(10) 1,3-Butanediol 5

(11) Maltol 1

(12)Raffinose 0.5

Surfactant (2% by mass)

(13) Sorbitan Isostearate 2

Solid or pasty oil (5% by mass)

(14) Paraffin 5

Purified water (12.7% by mass)

(15) Purified water 12.7

Oil agent

(16) Dimethicone (6cs) 3

(17) Methylphenyl polysiloxane 2

(18) Octyl p-methoxycinnamate 2

(19) Propylene glycol dicaprylate 2

(20) Dipentaerythritol hexahydroxystearate 0.5

Physiologically active ingredients

(21) Cranberry Extract 1

preservative

(22) Parabens 0.1

Comparative Example 10

Example 9 was otherwise completely repeated using the volatile cyclic pentameric siloxane instead of tetrakis(trimethylsiloxy)silane.

Comparative Example 11

Tetrakis(trimethylsiloxy)silane was used instead of purified water, and Example 9 was completely repeated (37.7% by mass of tetrakis(trimethylsiloxy)silane was mixed).

Comparative Example 12

Non-volatile dimethylpolysiloxane (10cs) was used instead of tetrakis(trimethylsiloxy)silane in Example 9, and Example 9 was repeated completely.

Comparative Example 13

Use liquid paraffin to replace the polyhydric alcohol of embodiment 9, other completely repeat embodiment 9.

Comparative Example 14

Use liquid paraffin to replace the paraffin of embodiment 9, other complete repetition embodiment 9.

Comparative Example 15

Example 9 was completely repeated except that the amount of paraffin wax in Example 9 was increased to 10% by mass while reducing the amount of purified water.

Comparative Example 16

Example 9 was completely repeated except that the amount of sorbitan isostearate in Example 9 was reduced to 1% by mass and the amount of purified water was increased.

Comparative Example 17

Example 9 was completely repeated except that the amount of sorbitan isostearate in Example 9 was increased to 5% by mass and the amount of purified water was increased.

Comparative Example 18

Example 9 was completely repeated except that the amount of purified water in Example 9 was made 0% by mass and the amount of 1,3-butanediol was increased.

Comparative Example 19

Purified water was used instead of tetrakis(trimethylsiloxy)silane in Example 9, and Example 9 was completely repeated.

Comparative Example 20

The pigment mixing amount of Example 9 was increased to 1.3 times (total amount of pigment: 9.66% by mass), and the amount of tetrakis (trimethylsiloxy) silane was reduced to 13.54% by mass, and the example was completely repeated 9.

Comparative Example 21

The pigment mixing amount of Example 9 was reduced to 1/4 (the total amount of pigment: 9.55% by mass), and the amount of tetrakis (trimethylsiloxy) silane was increased to 53.65% by mass, and the implementation was repeated completely Example 9.

The following skin effectiveness evaluations were performed on each foundation.

[Evaluation of effectiveness on skin]

For each evaluation item, invite 10 professional evaluators (the evaluators are sometimes repeated for different projects) to evaluate according to the evaluation criteria shown in the table below, and take the total score of the overall evaluators as the evaluation result. The higher the score, the higher the validity of the evaluation item. (full score: 50 points).

Evaluation criteria for skin effectiveness evaluation benchmark Fraction Feel the effect Feel the effect 54

Feel the effect a little bit 3

Only feel a little effect 2

Can't feel the effect 1

The evaluation results are shown below. Excellent skin affinity Attachment feels good Makeup lasts well Skin does not feel dry when applied no greasy feeling Example 9 ◎ ◎ ◎ ◎ ◎ Example 10 ◎ ◎ ◎ ◎ ◎ Comparative Example 10 ◎ ○ ◎ x ○ Comparative Example 11 △ △ ○ ◎ x Comparative Example 12 x x x ◎ x Comparative Example 13 x x △ ◎ x Comparative Example 14 x ○ △ ◎ ○ Comparative Example 15 x x x ◎ ○ Comparative Example 16 ○ △ △ ◎ △ Comparative Example 17 △ △ △ ◎ x Comparative Example 18 x x x x △ Comparative Example 19 x x ○ ◎ ○ Comparative Example 20 x x △ △ x Comparative Example 21 ○ ○ ○ ○ △

The stability of each foundation was evaluated by the following stability evaluation.

[Stability Evaluation]

The samples of Examples and Comparative Examples prepared according to the prescribed method were placed in a constant temperature bath at 0°C, 25°C, and 45°C for 3 weeks, and whether separation and aggregation were visible at any temperature was judged according to the following evaluation criteria. Storage stability was evaluated. benchmark evaluate No segregation coagulation Slight segregation coagulation Separation coagulation ○△×

The results are shown in the table below.

(formulation stability) Formulation Stability Example 9 Example 10 Comparative Example 10 Comparative Example 11 Comparative Example 12 Comparative Example 13 Comparative Example 14 Comparative Example 15 Comparative Example 16 Comparative Example 17 Comparative Example 18 Comparative Example 19 Comparative Example 20 Comparative Example 21 ○○○×△△×○△×××××

The results shown in the table above indicate that the examples of the present invention are superior in skin affinity, feeling, water resistance, sebum resistance, and formulation stability compared with the comparative examples. In Comparative Example 10, a volatile cyclic pentamer siloxane was used, and the examples were also excellent in greasy feeling and dry feeling. Comparative Example 11 is an example in which M4Q was used a lot, but it had an oily feeling, so the evaluation was poor.

Comparative Example 12 is an example when no volatile solvent is used, and it has a strong oily feeling and a sticky feeling, which is poor in feeling. Comparative Example 14 is an example in which solid oil was not used, and the viscosity was low, and there was a problem of overflowing from the container. Comparative Example 15 is an example in which many solid oils were used, and the preparation was hard and had a problem of caking. Comparative Example 16 is an example in which less surfactant was used, and there was a problem with the stability of the formulation. Comparative Example 17 is an example in which a lot of surfactants are used, and it has a problem in feeling. Comparative Example 18 is an example in which purified water was not used, and was poor in both stability and sensory evaluations. Comparative Example 19 is an example in which a lot of purified water was used, and there was a rough feeling and a sensory problem. Comparative Example 20 is an example in which the mixing amount of the pigment was increased, and the balance of the preparation was disturbed, and the evaluations of feeling and stability were poor. Comparative Example 21 is an example of reducing the amount of the pigment mixed, and the feeling is acceptable and balanced, but the balance of the preparation is broken, it is difficult to take it out from the container, and there is a problem with stability.

Embodiment 11: anti-ultraviolet make-up primer

A silicone resin trimethylsiloxysilicic acid was dissolved in tetrakis(trimethylsiloxy)silane at a concentration of 50% by mass to prepare a solution, and an anti-ultraviolet cosmetic primer was prepared according to the formula in the following table.

(Ingredient A) (%)

(1) Siloxane-treated titanium oxide particles 4

(2)Methyltris(trimethylsiloxy)silane 10

(3)Tetrakis(trimethylsiloxy)silane 15

(4) Polyether modified siloxane

(KF6017 manufactured by Shin-Etsu Chemical Co., Ltd.) 1

(ingredient B)

(5) Siloxane-treated zinc oxide particles 6

(6) Perfluoroalkyl Phosphate

Treated Flesh Colored Mica 0.5

(ingredient C)

(7) Cross-linked organopolysiloxane spherical powder (elastomer) 4

(8) Dimethicone (KF96A-6) 2

(9) Fluorinated dimethiconol 1

(10) Trimethylsiloxysilicic acid solution 6

(11) Octyl p-methoxycinnamate 3

(12) Perfluoropolyether 0.5

(ingredient D)

(13)Ethanol 10

(14) Purified water Balance

(15)Aloe Vera Extract 1

(16) Cranberry Extract 1

(17) Hibiscus extract 0.5

KF 6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

KF 96A-6 (manufactured by Shin-Etsu Chemical Co., Ltd.): Dimethicone with a viscosity of 6 mm ² /s

[preparation method]

Step 1: Grind component A with a roller mill to make a paste.

Step 2 Simply mix component C and grind it thoroughly with a mixer.

Step 3 Mix component B and component C, add component A after fully dispersed, and further mix thoroughly.

Step 4: Then add the uniformly dissolved component D, stir well, and then fill it into a container together with stainless steel beads to obtain a product.

Comparative Example 22

Using cyclic 6-mer volatile siloxane instead of tetrakis(trimethylsiloxy)silane, Example 11 was repeated completely.

Example 12

Example 11 was otherwise completely repeated using tetrakis(trimethylsiloxy)silane instead of methyltris(trimethylsiloxy)silane.

Comparative Example 23

Example 11 was otherwise completely repeated using methyltris(trimethylsiloxy)silane instead of tetrakis(trimethylsiloxy)silane.

Examples 13, 14 and 15: Daily Whitening Cream

Prepare the whitening cream according to the recipe below. As the mixed solvent, a 1:1 mixed solvent of tetrakis(trimethylsiloxy)silane and methyltris(trimethylsiloxy)silane was used. Example 13 14 15 (Component A) (%) (1) KF6017 (2) KF6026 (3) KF56 (4) KF995 (5) mixed solvent (component B) (6) glycerin (7) dipropylene glycol (8) p-hydroxybenzoic acid Methyl Ester (9) Sodium Ascorbyl Sulfate (10) Sodium Ascorbyl Phosphate (11) Gamma-Aminobutyric Acid (12) Apple Seed Core Extract (Antioxidant) (13) Sodium Chloride (14) Fragrance (15) Pure water 1-512105100.20.10.10.10.10.90.1 margin 1-53195100.20.10.10.10.10.90.1 margin 125-125100.20.10.10.10.10.90.1 margin

KF 6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

KF 6026 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene methyl siloxane polyoxypropylene oleyl methyl siloxane dimethyl siloxane copolymer (HLB=4.7)

KF 56 (manufactured by Shin-Etsu Chemical Co., Ltd.): Methylphenylpolysiloxane

KF 995 (manufactured by Shin-Etsu Chemical Co., Ltd.): Decamethylcyclopentasiloxane (D5)

[preparation method]

Step 1 Heat and dissolve component A at 60°C.

Step 2 Heat and dissolve component B at 60°C.

Step 3 Add ingredient A to ingredient B while stirring, emulsify and mix.

Step 4 Next, cool down to 30°C while stirring, and fill it into a container to make a product.

Comparative Example 24

Example 14 was repeated except that ethanol was used instead of the mixed solvent of Example 14.

Comparative Example 25

Example 15 was repeated except that light liquid paraffin was used instead of the mixed solvent of Example 15.

Comparative Example 26

Tetrakis(trimethylsiloxane) containing 35% of 1,1,1,5,5,5-hexamethyl-3-trimethylsiloxy-3-hydroxytrisiloxane prepared in Preparation Comparative Example 1 was used. Siloxy)silane was used instead of the mixed solvent of Example 15, and Example 15 was all repeated except that.

Comparative Example 27

Tetrakis(trimethylsiloxane) containing 35% of 1,1,1,5,5,5-hexamethyl-3-trimethylsiloxy-3-hydroxytrisiloxane prepared in the comparative example above Siloxy)silane and tetrakis(trimethylsiloxy)silane were mixed to obtain 5% 1,1,1,5,5,5-hexamethyl-3-trimethylsiloxy-3- Tetrakis(trimethylsiloxy)silane of hydroxytrisiloxane was used instead of the mixed solvent of Example 15, and Example 15 was repeated except for this.

Example 16: Sunscreen

Sunscreens were prepared according to the formulations below. The anti-ultraviolet component adopts 2-ethylhexyl p-methoxycinnamate, treated titanium oxide particles, treated zinc oxide particles, and treated yellow titanium oxide particles, and uses trimethylsiloxysilicic acid as the siloxane resin.

Titanium oxide microparticles were treated by coating titanium oxide microparticles coated with aluminum silicate having an average particle diameter of 17 nm with octyltrimethoxysilane in a coating amount of 8% by mass, followed by heat treatment at 160°C. Zinc oxide microparticles were treated by coating silica-treated zinc oxide microparticles having an average particle diameter of 50 nm with methylhydrogenpolysiloxane in a coating amount of 3% by mass, followed by heat treatment at 170°C. The treatment of the yellow titanium oxide fine particles used the following: silica-treated iron-doped titanium oxide fine particles were coated with methylhydrogenpolysiloxane in a coating amount of 3% by mass, and heat-treated at 130°C.

(Ingredient A) (%)

Treatment of titanium oxide particles 8.0

Tetrakis(trimethylsiloxy)silane 9.0

Methyltris(trimethylsiloxy)silane 3.0

(ingredient B)

Treatment of yellow titanium oxide particles 0.8

Handling Zinc Oxide Particles 12.0

(ingredient C)

Stereo-crosslinked organopolysiloxane spherical powder (elastomer) 1.0

Dimethiconol 6.0

Tetrakis(trimethylsiloxy)silane 15.0

Trimethylsiloxysilicic acid 6.0

2-Ethylhexyl p-methoxycinnamate 10.0

(ingredient D)

Ethanol 13.0

Purified water Balance

Aloe Vera Extract 0.5

Component A was pulverized with a roller mill to prepare a paste. Component C is simply mixed and pulverized sufficiently with a mixer. Component B and component C are mixed and dispersed well, then component A is added, and further mixed well. Then add the uniformly dissolved component D, stir well, and then fill it into a container together with stainless steel beads to obtain a product.

Comparative Example 28

Use linear tetramer volatile siloxane instead of tetrakis(trimethylsiloxy)silane, and repeat Example 16 otherwise.

Example 17

Example 16 was otherwise completely repeated using tetrakis(trimethylsiloxy)silane instead of methyltris(trimethylsiloxy)silane.

Comparative Example 29

Example 16 was otherwise completely repeated using methyltris(trimethylsiloxy)silane instead of tetrakis(trimethylsiloxy)silane.

Embodiment 18: sunscreen (cream)

(Element) (%)

(1)Methyltris(trimethylsiloxy)silane 3.0

(2)Tetrakis(trimethylsiloxy)silane 17.0

(3) Liquid paraffin 10.0

(4)KF6017 1.9

(5)KF6026 4.0

(6) 4-tert-butyl-4'-methoxydibenzoylmethane 7.0

(7) Distearyldimethylammonium chloride 0.8

(8) Vitamin E acetate 0.1

(9)Ethanol 1.0

(10) Green Soil 1.2

(11) Preservatives Appropriate amount

(12) Spices Appropriate amount

(13) Purified water Balance

KF 6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

KF 6026 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene methyl siloxane polyoxypropylene oleyl methyl siloxane dimethyl siloxane copolymer (HLB=4.7)

[Preparation]

A: Ingredients (1)-(8) and (11) are heated and mixed.

B: Components (9), (10) and (13) are heated and uniformly dispersed and mixed.

C: Slowly add B to A under stirring, emulsify, cool, add component (12), and obtain a sunscreen (cream).

Embodiment 19: sunscreen (cream)

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 18.0

(2)KF56 2.0

(3) Liquid paraffin 1.5

(4)KF6012 4.0

(5) Octyl p-methoxycinnamate 5.0

(6) 1,3-Butanediol 4.0

(7) Sodium chloride 1.0

(8) Preservatives Appropriate amount

(9) Spices Appropriate amount

(10) Appropriate amount of purified water

KF 56 (manufactured by Shin-Etsu Chemical Co., Ltd.): Methylphenylpolysiloxane

KF 6012 (manufactured by Shin-Etsu Chemical Co., Ltd.): Polyoxyethylene-polyoxypropylene-methylpolysiloxane copolymer (HLB=7.0)

[Preparation]

A: Components (1)-(6) are heated and mixed.

B: Components (7)-(9) and (11) are heated and dissolved.

C: Slowly add B to A under stirring, emulsify, cool, add component (10), and obtain a sunscreen (cream).

Embodiment 20: sunscreen (cream)

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 16.5

(2)Methyltris(trimethylsiloxy)silane 1.0

(3)KP 545 12.0

(4) Glyceryl triethylhexanoate 5.0

(5) Octyl p-methoxycinnamate 6.0

(6) KSG 21 5.0

(7)KF6017 1.0

(8) Lipophilic treatment of zinc oxide 20.0

(9) Sodium chloride 0.5

(10) 1,3-Butanediol 2.0

(11) Preservatives Appropriate amount

(12) Spices Appropriate amount

(13) Purified water Balance

KF 545 (manufactured by Shin-Etsu Chemical Co., Ltd.): acrylic siloxane copolymer resin/decamethylcyclopentasiloxane 30% solution

KSG 21 (manufactured by Shin-Etsu Chemical Co., Ltd.): Cross-linked polyether-modified methylpolysiloxane/dimethylpolysiloxane

KF 6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

[Preparation]

A: The component (3) was added to a part of the component (1) to make it uniform, and the component (8) was added and dispersed with a bead mill.

B: Mix (2) and (4)-(7) with the remaining component (1), and mix uniformly.

C: Components (9)-(11) and (13) are mixed and dissolved.

D: Add C to B, emulsify, add A and component (12), and obtain a sunscreen (cream).

Embodiment 21: Sunscreen (lotion)

(Element) (%)

(1)Methyltris(trimethylsiloxy)silane 13.0

(2)Tetrakis(trimethylsiloxy)silane 1.0

(3)KF 615A 10.0

(4) Squalane 1.5

(5) Octyl p-methoxycinnamate 3.0

(6) Titanium TT0-S2 2.0

(7) Polymethylsilsesquioxane 0.7

(8) 1,3-Butanediol 10.0

(9) Sodium chloride 2.0

(10)L-proline 0.1

(11) 2-Hydroxycaprylic acid 1.0

(12) 2-Hydroxypropionic acid 5.0

(13) Sodium hydroxide Appropriate amount

(14) Preservatives Appropriate amount

(15) Spices Appropriate amount

(16) Purified water Balance

KF 615A (manufactured by Shin-Etsu Chemical Co., Ltd.): Polyoxyethylene-polyoxypropylene-methylpolysiloxane copolymer (HLB=14.0)

Titanium TTO-S2 (product made in Ishihara industry company): Hydrophobization treatment titanium oxide ultrafine particles

[Preparation]

A: Components (8)-(16) are uniformly dissolved.

B: Components (1)-(5) are mixed, and components (6) and (7) are added to make it uniform.

Embodiment 22: sunscreen (emulsion)

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 25.0

(2) diglyceryl monoisostearate 1.5

(3) Decacylglycerol Pentaisostearate 1.5

(4)KF 6012 0.5

(5) Olive oil 1.0

(6) Titanium oxide particles 7.0

(7) Glycerin 5.0

(8) Sodium chloride 1.5

(9) Preservatives Appropriate amount

(10) Spices Appropriate amount

(11) Purified water Balance

KF 6012 (manufactured by Shin-Etsu Chemical Co., Ltd.): Polyoxyethylene-polyoxypropylene-methylpolysiloxane copolymer (HLB=7.0)

[Preparation]

A: Heat and mix ingredients (1)-(5) to uniformly disperse ingredient (6).

B: Ingredients (7)-(9) and (11) are heated and mixed.

C: Slowly add B to A under stirring, emulsify, cool, add component (10), and obtain a sunscreen (emulsion).

Embodiment 23: sunscreen (emulsion)

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 15.0

(2) Ethanol 5.0

(3)KF 56 3.0

(4) Sorbitan monoisostearate 1.0

(5)KF 6012 0.5

(6) Silicone resin 1.0

(7) Octyl p-methoxycinnamate 4.0

(8) Titanium oxide particles 8.0

(9) Sorbitol 2.0

(10) Sodium chloride 2.0

(11) Preservatives Appropriate amount

(12) Spices Appropriate amount

(13) Purified water Balance

KF 56 (manufactured by Shin-Etsu Chemical Co., Ltd.): Methylphenylpolysiloxane

Silicone resin: 50% methyltris(trimethylsiloxane) of a siloxane network compound (trimethylsiloxysilicic acid) with a [Me ₃ SiO _1/2 ]/[SiO ₂ ] ratio of 0.8 base) silane solution

KF 6012 (manufactured by Shin-Etsu Chemical Co., Ltd.): Polyoxyethylene-polyoxypropylene-methylpolysiloxane copolymer (HLB=7.0)

[Preparation]

A: Components (1)-(7) are heated and mixed, and component (8) is uniformly dispersed.

B: Components (9)-(11) and (13) are heated and mixed.

C: Slowly add B to A under stirring, emulsify, cool, add component (12), and obtain a sunscreen (emulsion).

The evaluation results of the above-mentioned Examples 11-23 and Comparative Examples 22-29 are shown in the table below. Non-irritating to the skin when applied Good smudge Easy to use as a makeup base Skin is not rough after application ○Example 11 Comparative Example 22 Example 12 Comparative Example 23 ○Daily Whitening Cream Example 13 Example 14 Example 15 Comparative Example 24 Comparative Example 25 Comparative Example 26 Comparative Example 27 ○Sunscreen Example 16 Comparative Example 28 Example 17 Comparative Example 29 Example 18 Example 19 Example 20 Example 21 Example 22 Example 23 464246454443421011101039184344444441394239 433437354142411929101037203330384140394042 453546404044401013101039123732384340444141 504450364849484048101043264633474644404846

The evaluation results showed that the examples of the present invention showed excellent performance in any of the evaluation items. Compared with the comparative examples, the examples not only have less dry feeling, but also have good spreadability and have a moderate moist feeling, which is excellent in terms of feeling. And the anti-ultraviolet effect of the embodiment of the present invention is excellent. The results of comparative examples 26 and 27 show that: 1,1,1,5,5,5-hexamethyl-3-trimethylsiloxy-3-hydroxytrisiloxane is more, and the sensory and safety aspects has a problem. From the results of Comparative Example 28, it can be seen that the linear volatile siloxane irritated the skin and gave a poor feeling.

Example 24: Suntan Cream

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 12.0

(2)Methyltris(trimethylsiloxy)silane 3.0

(3)KF 96A-100 5.0

(4)KP-562 0.5

(5) Branched chain siloxane type polyglycerol modified siloxane 2.2

(HLB=5)

(6)KF 6026 6.0

(7) Palmitic acid 0.2

(8)Dimethyloctyl p-aminobenzoate 0.5

(9) 4-tert-butyl-4'-methoxydibenzoylmethane 0.5

(10) Kaolin 0.5

(11) Iron oxide red 0.2

(12) Iron oxide yellow 0.3

(13) Iron oxide black 0.1

(14) Mica coated with titanium oxide 1.0

(15) L-sodium glutamate 3.0

(16) 1,3-Butanediol 5.0

(17)Dioctadecyldimethylammonium chloride 0.1

(18) Antioxidants Appropriate amount

(19) Preservatives Appropriate amount

(20) Spices Appropriate amount

(21) Purified water Balance

KF 96A-100 (manufactured by Shin-Etsu Chemical Co., Ltd.): dimethyl polysiloxane with a viscosity of 100 mm ² /s

KP-562 (manufactured by Shin-Etsu Chemical Co., Ltd.): behenyl-modified acrylic siloxane graft copolymer

KF 6026 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene methyl siloxane polyoxypropylene oleyl methyl siloxane dimethyl siloxane copolymer (HLB=4.7)

[Preparation]

A: Components (1)-(9) and (18)-(19) are heated and dissolved.

B: Component (17) and a part of (21) are heated and stirred, and then components (10)-(14) are added and dispersed.

C: The remainder of ingredients (15)-(16) and (21) are uniformly dissolved and mixed with B.

D: Slowly add C to A under stirring, emulsify, cool, add component (20), and obtain a tanning cream.

It can be seen that the suntan lotion obtained above has no change with temperature or time such as separation or powder aggregation, and has excellent stability, good spreadability, and moderate moist feeling.

Example 25: Foundation

(Element) (%)

(1)Methyltris(trimethylsiloxy)silane 30.0

(2)Tetrakis(trimethylsiloxy)silane 15.0

(3)KF 96A-6 5.0

(4)KF 6017 1.5

(5)KF 6026 0.5

(6) Octadecyldimethylbenzyl ammonium salt modified montmorillonite 4.0

(7) Hydrophobic treatment of titanium oxide* 10.0

(8) Hydrophobic treated talc* 6.0

(9) Hydrophobic treated mica* 6.0

(10) Hydrophobic treatment red iron oxide* 1.6

(11) Hydrophobic treatment of iron oxide yellow* 0.7

(12) Hydrophobic treated iron oxide black* 0.2

(13) Dipropylene Glycol 5.0

(14) Methylparaben 0.3

(15) 2-Amino-2-methyl-1,3-propanediol 0.2

(16) Hydrochloric acid 0.1

(17) Spices Appropriate amount

(18) Purified water Balance

KF 96A-100 (manufactured by Shin-Etsu Chemical Co., Ltd.): dimethyl polysiloxane with a viscosity of 100 mm ² /s

KF 6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

KF 6026 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene methyl siloxane polyoxypropylene oleyl methyl siloxane dimethyl siloxane copolymer (HLB=4.7)

*: Hydrophobic treated powder: Added 2% of methyl hydrogen polysiloxane to the powder, followed by heat treatment.

(Preparation)

A: Components (1)-(6) are heated and mixed, and components (7)-(12) are added to make it uniform.

B: Components (13)-(16) and (18) are heated and dissolved. (The pH of the water system is 9.0).

C: Slowly add B to A under stirring, emulsify, cool, add component (17), and obtain a foundation.

The foundation obtained as described above has no changes such as separation with temperature or time, or powder aggregation, and is not only excellent in stability, but also has good makeup durability.

Example 26: Foundation

(Element) (%)

(1)KF 96A-6 5.0

(2)Tetrakis(trimethylsiloxy)silane 4.0

(3) Methyltris(trimethylsiloxy)silane 11.0

(4) Squalane 4.0

(5) Neopentyl glycol dicaprylate 3.0

(6) Diglyceryl Isostearate Myristate 2.0

(7) α-Monoisostearyl Glyceryl Ether 1.0

(8)KF 6015 1.0

(9) Aluminum distearate 0.2

(10) Hydrophobic treatment of titanium oxide* 5.0

(11) Hydrophobic treated sericite* 2.0

(12) Hydrophobic treated talc* 3.0

(13) Hydrophobic treated iron oxide red* 0.4

(14) Hydrophobic treatment of iron oxide yellow* 0.7

(15) Hydrophobic treated iron oxide black* 0.1

(16)Magnesium sulfate 0.7

(17) Glycerin 3.0

(18) Preservatives Appropriate amount

(19) Spices Appropriate amount

(20) Purified water Balance

KF 6015 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.5)

*: Hydrophobic treated powder: Powder treated with 2% stearic acid

[Preparation]

A: Components (1)-(9) are heated and mixed, and components (10)-(15) are added to make it uniform.

B: Components (16)-(18) and (20) are heated and dissolved.

C: Slowly add B to A under stirring, emulsify, cool, add component (19) to obtain a foundation.

The foundation obtained as described above has no changes such as separation with temperature or time, or powder aggregation, and is not only excellent in stability, but also has good makeup durability.

Example 27: Foundation

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 15.0

(2)Methyltris(trimethylsiloxy)silane 3.0

(3)KF 56 5.0

(4) Sorbitan monoisostearate 0.5

(5) diglyceryl monoisostearate 0.5

(6)KF 6012 1.0

(7) Octyl p-methoxycinnamate 3.0

(8) Titanium oxide 10.0

(9) Iron oxide red 0.13

(10) Iron oxide yellow 0.3

(11) Iron oxide black 0.07

(12) Talc 2.5

(13) Sorbitol 2.0

(14)Magnesium sulfate 0.1

(15)Ethanol 10.0

(16) Preservatives Appropriate amount

(17) Spices Appropriate amount

(18) Purified water Balance

KF 56 (manufactured by Shin-Etsu Chemical Co., Ltd.): Methylphenylpolysiloxane

KF 6012 (manufactured by Shin-Etsu Chemical Co., Ltd.): Polyoxyethylene-polyoxypropylene-methylpolysiloxane copolymer (HLB=7.0)

[Preparation]

A: The ingredients (8)-(12) are mixed uniformly.

B: Heat and mix ingredients (1)-(7) and (16), add A, disperse and mix evenly.

C: Ingredients (13)-(14) and (18) are heated, added to B and emulsified, cooled, and ingredients (15) and (17) are added to obtain a foundation.

The foundation obtained as described above has a good emulsification state, is not affected by temperature, does not separate or aggregate over time, and has excellent stability.

Example 28: Foundation

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 15.0

(2)KF 96A-6 5.0

(3) Liquid paraffin 3.0

(4)KF 6015 3.0

(5) Palmitic acid 0.5

(6) アエロジル RY20 5.0

(7) Titanium oxide 6.0

(8) Iron oxide red 0.25

(9) Iron oxide yellow 0.6

(10) Iron oxide black 0.12

(11) Sericite 8.03

(12) Dipropylene Glycol 10.0

(13) Magnesium Sulfate 2.0

(14) Preservatives Appropriate amount

(15)Antioxidants Appropriate amount

(16) Spices Appropriate amount

(17) Purified water Balance

KF 96A-6 (manufactured by Shin-Etsu Chemical Co., Ltd.): Dimethicone with a viscosity of 6 mm ² /s

KF 6015 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.5)

Aerosil RY200 (manufactured by Aerosil Corporation of Japan): Hydrophobic silica

(Preparation)

A: The ingredients (7)-(12) are mixed uniformly.

B: Heat and mix ingredients (1)-(6) and (16) at 70°C, add A, and disperse and mix evenly.

C: Components (13)-(15) and (18) were heated at 70° C., added to B and emulsified, cooled, and component (17) was added to obtain a foundation.

It can be seen that the emulsified state of the foundation obtained as described above is good, it is excellent in makeup durability, it is not much affected by temperature, and it is very excellent in stability over time.

Example 29: Foundation

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 9.0

(2) Decamethylcyclopentasiloxane 3.0

(5)Methyltris(trimethylsiloxy)silane 3.0

(6)KF 96A-6 8.0

(7) Octyl p-methoxycinnamate 3.0

(8) 12-Hydroxystearic Acid 1.0

(9)FL-100 15.0

(10)FPD-6131 5.0

(11)KMP 590 3.0

(12) Fluorine compound treated titanium oxide particles* 8.0

(13) Fluorine compound treated mica titanium* 1.0

(14) Fluorine compound treated titanium oxide* 5.0

(15) Fluorine compound treated iron oxide red* 0.9

(16) Fluorine compound treated iron oxide yellow* 2.0

(17) Fluorine compound treated iron oxide black* 1.0

(18)Ethanol 15.0

(19) Glycerin 3.0

(20)Magnesium sulfate 1.0

(21) Preservatives Appropriate amount

(22) Spices Appropriate amount

(23) Purified water Surplus

KF 96A-6 (manufactured by Shin-Etsu Chemical Co., Ltd.): Dimethicone with a viscosity of 6 mm ² /s

FL-100 (manufactured by Shin-Etsu Chemical Co., Ltd.): Trifluoropropylmethylsiloxane

FPD-6131 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-trifluoropropyl-methylpolysiloxane copolymer (HLB=5.4)

KMP 590 (manufactured by Shin-Etsu Chemical Co., Ltd.): spherical silicone resin powder

*: Fluorine compound treated powder: coated with 5% perfluoroalkyl ethyl phosphate diethanolamine salt

[Preparation]

A: Ingredients (10)-(16) are mixed uniformly.

B: Heat and mix components (1)-(9) at 70°C, add A, disperse and mix evenly.

C: The components (17)-(20) and (22) were heated at 40°C, slowly added to B and emulsified, cooled, and the component (21) was added to obtain a liquid foundation.

The foundation obtained as described above does not change with temperature or time, and has excellent stability.

Example 30: Foundation

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 27.0

(2)KF 56 3.0

(3) Glyceryl triethylhexanoate 10.0

(4)KF 6017 1.0

(5)KF 6026 1.0

(6) Polyglyceryl Monoisostearate 3.0

(7) Hydrophobic treatment mixed powder (Note 1) 18.0

(8) Iron oxide red 1.2

(9) Iron oxide yellow 2.6

(10) Iron oxide black 0.2

(11) 1,3-Butanediol 7.0

(12) Sodium chloride 0.5

(13) Preservatives Appropriate amount

(14) Spices Appropriate amount

(15) Purified water Balance

(Note 1) Hydrophobic treatment mixed powder

a) Siloxane-treated titanium oxide particles 8.0

b) Siloxane treatment of zinc oxide particles 4.0

c) Silicone treated talc 3.0

d) Silicone treated mica 3.0

KF 56 (manufactured by Shin-Etsu Chemical Co., Ltd.): Methylphenylpolysiloxane

KF 6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

KF 6026 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene methyl siloxane polyoxypropylene oleyl methyl siloxane dimethyl siloxane copolymer (HLB=4.7)

[Preparation]

A: Mix ingredients a-d.

B: Components (1)-(6) are mixed, heated and dissolved, and components (7)-(10) are uniformly dispersed.

C: Ingredients (11)-(13) and (15) are mixed, then added to B for emulsification.

D: Cool C, add component (14), and obtain a foundation.

The foundation obtained as described above has excellent adhesion, glossy makeup, very excellent makeup durability, and excellent stability without changing with temperature or time.

Example 31: Hair Cream

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 9.0

(2) Methyltris(trimethylsiloxy)silane 1.0

(3)KF 56 4.0

(4) Squalane 5.0

(5) Silicone resin 1.0

(6) Glyceryl dioleate 2.0

(7)KF 6017 2.0

(8)KF 6026 4.0

(9) Sodium sorbitol sulfate 2.0

(10) Sodium chondroitin sulfate 1.0

(11) Sodium Hyaluronate 0.5

(12) Propylene Glycol 3.0

(13) Preservatives 1.5

(14) Vitamin E acetate 0.1

(15) Antioxidants Appropriate amount

(16) Spices Appropriate amount

(17) Purified water Balance

KF 56 (manufactured by Shin-Etsu Chemical Co., Ltd.): Methylphenylpolysiloxane

Silicone resin: 50% methyltris(trimethylsiloxane) of a siloxane network compound (trimethylsiloxysilicic acid) with a [Me ₃ SiO _1/2 ]/[SiO ₂ ] ratio of 0.8 base) silane solution

KF 6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

KF 6026 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene methyl siloxane polyoxypropylene oleyl methyl siloxane dimethyl siloxane copolymer (HLB=4.7)

(Preparation)

A: Ingredients (1)-(8) and (13)-(14) are heated and mixed.

B: Components (9)-(12) and (17) are heated and dissolved.

C: Slowly add B to A under stirring, emulsify, cool, add component (16), and obtain a hair cream.

The hair cream obtained as described above has good durability, does not change with temperature or time, and is also excellent in stability.

Example 32: Mascara

(Element) (%)

(1)KP 545 20.0

(2) Dextrin Palmitate/Ethylhexanoate 8.0

(3) Polyethylene wax 4.0

(4) Beeswax 7.0

(5) Lecithin 0.5

(6)Methyltris(trimethylsiloxy)silane The balance

(7)Tetrakis(trimethylsiloxy)silane 5.0

(8) Isododecane 20.0

(9) Iron oxide 5.0

(10) アエロジル RY200 3.5

(11) Talc 10.0

KP 545 (manufactured by Shin-Etsu Chemical Co., Ltd.): acrylic siloxane copolymer resin/decamethylcyclopentasiloxane 30% solution

Aerosil RY200 (manufactured by Japan Aerosil Corporation): hydrophobized silica

[Preparation]

A: Mix and dissolve ingredients (1)-(8).

B: Components (9)-(11) are added to A and dispersed with a roller.

The mascara obtained as described above has good durability, does not change with temperature or time, and is also excellent in stability.

Example 33: Skin Cream

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 20.0

(2) Glyceryl tricaprylate 10.0

(3)KF 6017 1.5

(4)KF 6026 4.0

(5) Phenyldimethylstearyl ammonium chloride 1.0

(6) 1,3-Butanediol 10.0

(7) Maltol 10.0

(8) Soapstone 1.5

(9) Preservatives Appropriate amount

(10) Spices Appropriate amount

(12) Purified water Balance

KF6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

KF 6026 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene methyl siloxane polyoxypropylene oleyl methyl siloxane dimethyl siloxane copolymer (HLB=4.7)

[Preparation]

A: Components (1)-(5) and (9) are heated and mixed.

B: Components (6)-(8) and (11) are heated and dissolved.

C: Slowly add B to A under stirring, emulsify, cool, add component (10), and obtain cream.

The cream obtained as described above has good durability, does not change with temperature or time, and is also excellent in stability.

Example 34: Skin Cream

A mixed solution of methyltris(trimethylsiloxy)silane (M3T) and tetrakis(trimethylsiloxy)silane (M4Q) mixed at 1:1 was used as the mixed solution.

(Element) (%)

(1) Mixed solution 10.0

(2)KF 96A-6 5.0

(3) Liquid paraffin 5.0

(4) Water-dispersed silicone elastomer spherical powder 2.0

(5)KF 6017 3.0

(6)KF 6026 5.0

(7) Sodium citrate 2.0

(8) 1,3-Butanediol 5.0

(9) Preservatives Appropriate amount

(10) Spices Appropriate amount

(11) Purified water Balance

KF 96A-6 (manufactured by Shin-Etsu Chemical Co., Ltd.): Dimethicone with a viscosity of 6 mm ² /s

KF 6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

KF 6026 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene methyl siloxane polyoxypropylene oleyl methyl siloxane dimethyl siloxane copolymer (HLB=4.7)

[Preparation]

A: Heat and mix ingredients (1)-(5).

B: Components (6)-(9) and (11) are heated and dissolved.

C: Slowly add B to A under stirring, emulsify, cool, add component (10), and obtain cream.

The cream obtained as described above has a moderate moist feeling, is long-lasting, does not change with temperature or time, and is also excellent in stability.

Example 35: Skin Cream

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 20.0

(2) Liquid paraffin 5.0

(3)KF 615A 1.0

(4) Magnesium L-Ascorbyl Phosphate 3.0

(5) Dipropylene Glycol 5.0

(6) Glycerin 5.0

(7) Preservatives Appropriate amount

(8) Spices Appropriate amount

(9) Purified water Balance

KF 615A (manufactured by Shin-Etsu Chemical Co., Ltd.): Polyoxyethylene-polyoxypropylene-methylpolysiloxane copolymer (HLB=14.0)

[Preparation]

A: The ingredients (1)-(3) are uniformly mixed.

B: Components (5)-(7) are heated to make them uniform.

C: Components (4) and (9) are uniformly dissolved.

D: Under stirring, slowly add B to A, then add C, emulsify, add component (8), and obtain cream.

The cream thus obtained is easily compatible with the skin, does not change with temperature or time, and has excellent stability.

Example 36: Skin Cream

A mixed solution in which methyltris(trimethylsiloxy)silane and tetrakis(trimethylsiloxy)silane were mixed in a ratio of 7:3 was used as the mixed solution.

(Element) (%)

(1) Mixed solution 20.0

(2)KF 56 5.0

(3)KF 6012 1.5

(4) Dextrin fatty acid ester 1.0

(5) Glycerin 5.0

(6) Sodium chloride 1.0

(7) Preservatives Appropriate amount

(8) Spices Appropriate amount

(9) Purified water Balance

KF 56 (manufactured by Shin-Etsu Chemical Co., Ltd.): Methylphenylpolysiloxane

KF 6012 (manufactured by Shin-Etsu Chemical Co., Ltd.): Polyoxyethylene-polyoxypropylene-methylpolysiloxane copolymer (HLB=7.0)

[Preparation]

A: The ingredients (1)-(4) are heated and mixed.

B: Dissolve (5)-(7) and (9) by heating.

C: Slowly add B to A under stirring, emulsify, cool, add component (8), and obtain cream.

The usability of the cream obtained as described above was very good. In addition, it is excellent in water resistance and perspiration resistance, maintains makeup well, does not change with temperature or time, and has excellent stability.

Example 37: Skin Cream

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 18.0

(2)KF 96A-100 2.0

(3) Polypropylene glycol (3) Myristyl ether 0.5

(4)KF 6017 1.4

(5)KF 6026 2.5

(6) Hydrophobic treatment of titanium oxide particles* 1.0

(7) Glycerin 3.0

(8) 70% Sorbitol 5.0

(9) Citric acid 25.0

(10) Sodium chloride 0.6

(11) Preservatives Appropriate amount

(12) Spices Appropriate amount

(13) 32% ammonia water 4.5

(14) Purified water Balance

KF 96A-100 (manufactured by Shin-Etsu Chemical Co., Ltd.): dimethyl polysiloxane with a viscosity of 100 mm ² /s

KF 6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

KF 6026 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene methyl siloxane polyoxypropylene oleyl methyl siloxane dimethyl siloxane copolymer (HLB=4.7)

*: Hydrophobic treated titanium oxide fine particles: Aluminum stearate treated titanium oxide fine particles

[Preparation]

A: Mix ingredients (1)-(5) and (12), then mix ingredient (6) and stir.

B: Components (7)-(11) and (13)-(14) are uniformly dissolved.

C: Slowly add B to A to emulsify to obtain a cream.

The cream obtained as described above had good spreadability during application despite containing a large amount of citric acid, did not change with temperature or time, and was excellent in stability.

Example 38: Skin Cream

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 15.0

(2) Decamethylcyclopentasiloxane 1.0

(3)KF 96A-6 4.0

(4)KF 6012 5.0

(5)POE(5)octyl dodecyl ether 1.0

(6) Polyoxyethylene sorbitan monostearate (20E.O.) 0.5

(7) サンスフエア SZ-5 4.0

(8) Siloxane-treated titanium oxide particles 5.0

(9) Liquid paraffin 2.0

(10) Macadamia Oil 1.0

(11) Scutellaria baicalensis extract* 1.0

(12) Gentian extract** 0.5

(13)Ethanol 5.0

(14) 1,3-Butanediol 2.0

(15) Preservatives Appropriate amount

(16) Spices Appropriate amount

(17) Purified water Balance

KF 96A-6 (manufactured by Shin-Etsu Chemical Co., Ltd.): Dimethicone with a viscosity of 6 mm ² /s

KF 6012 (manufactured by Shin-Etsu Chemical Co., Ltd.): Polyoxyethylene-polyoxypropylene-methylpolysiloxane copolymer (HLB=7.0)

Sunsufea SZ-5 (manufactured by Asahi Glass Co.): Zinc oxide treated with silicic anhydride; silicon dioxide with a particle size of 0.01-10 μm containing 50% zinc oxide;

*: Scutellaria baicalensis extract: extracted with 50% 1,3-butanediol water

**: Gentian extract: extracted with 20% ethanol water

[Preparation]

A: Mix and disperse ingredients (7)-(10) uniformly.

B: Mix ingredients (1)-(6) and add A.

C: Mix components (11)-(15) and (17), then add B and emulsify.

D: Cool C, add component (16), and obtain cream.

The cream obtained as described above has excellent adhesion, glossy makeup, very excellent makeup retention, and excellent stability without changes with temperature or time.

Example 39: Hand cream

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 1.0

(2) Methyltris(trimethylsiloxy)silane 11.0

(3) Alpha olefin oligomers 10.0

(4) Silicone resin 5.0

(5)KF 6017 1.9

(6)KF 6026 4.0

(7) Distearyldimethylammonium chloride 0.8

(8) Vitamin E acetate 0.1

(9) Macrogol 4000 1.0

(10) Glycerin 10.0

(11) Green Soil 1.2

(12) Preservatives Appropriate amount

(13) Spices Appropriate amount

(14) Purified water Balance

Silicone resin: 70% methyltris(trimethylsiloxane) of a siloxane network compound (trimethylsiloxysilicic acid) with a [Me ₃ SiO _1/2 ]/[SiO ₂ ] ratio of 1.15 base) silane solution

KF 6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

KF 6026 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene methyl siloxane polyoxypropylene oleyl methyl siloxane dimethyl siloxane copolymer (HLB=4.7)

[Preparation]

A: Components (1)-(8) and (12) are heated and mixed.

B: Dissolve (9)-(11) and (14) by heating.

C: Slowly add B to A under stirring, emulsify, cool, add component (13), and obtain a hand cream.

The coating film retention property of the hand cream obtained as above is good, it does not change with temperature or time, and it is also excellent in stability.

Example 40: Hand cream

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 30.0

(2) Liquid paraffin 10.0

(3) Amino-modified silicone rubber 15.0

(4)KF 6017 4.0

(5) Distearyldimethylammonium chloride 0.8

(6) Vitamin B acetate 0.1

(7) Macrogol 4000 1.0

(8) Glycerin 10.0

(9) Green Soil 1.2

(10) Preservatives Appropriate amount

(11) Spices Appropriate amount

(12) Purified water Balance

Amino modified silicone rubber: amine equivalent 70000g/mol

KF 6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

[Preparation]

A: Components (1), (3) are mixed and dissolved by heating, and components (2), (4)-(6), (10) are added by heating.

B: Ingredients (7)-(9) and (12) are heated and mixed.

C: After slowly adding B to A, emulsifying, cooling, and adding component (11), hand cream was obtained.

The hand cream obtained as described above can effectively protect the skin of a person engaged in washing work, and is very excellent in temperature stability.

Example 41: Hand Cream (O/W)

(Element) (%)

(1)KP 545 5.0

(2)Tetrakis(trimethylsiloxy)silane 4.5

(3)Methyltris(trimethylsiloxy)silane 0.5

(4)KSG 16 2.5

(5) Alpha Olefin Oligomers 5.0

(6) Vaseline 5.0

(7) Glyceryl triethylhexanoate 3.0

(8)KF 6017 0.5

(9) Polyoxyethylene sorbitan monooleate 1.0

(10) セピゲル 305 2.0

(11) 1,3-Butanediol 5.0

(12) Glycerin 5.0

(13) Preservatives Appropriate amount

(14) Spices Appropriate amount

(15) Purified water Balance

KP 545 (manufactured by Shin-Etsu Chemical Co., Ltd.): acrylic siloxane copolymer resin/decamethylcyclopentasiloxane 30% solution

KSG 16 (manufactured by Shin-Etsu Chemical Co., Ltd.): Crosslinked Dimethicone/Dimethicone

KF 6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

Sepigel 305: light liquid isoparaffin (manufactured by SEPPIC)

[Preparation]

A: The ingredients (1)-(8) are uniformly mixed.

B: Ingredients (9)-(12) and (14) are uniformly mixed.

C: Add B to A, emulsify, add component (13), and obtain O/W hand cream.

The hand cream obtained as described above has excellent adhesion, glossy makeup, very excellent makeup retention, and very excellent stability over temperature and time.

Example 42: Hand Cream (O/W)

(Element) (%)

(1)KP 545 5.0

(2)Tetrakis(trimethylsiloxy)silane 4.0

(3) Decamethylcyclopentasiloxane 1.0

(4)KP 561 8.0

(5) Cetyl Alcohol 1.0

(6) Glyceryl triisostearate 5.0

(7) Stearic acid 3.0

(8) Glyceryl monostearate 1.5

(9)KF 6015 0.7

(10)Sorbitan sesquioleate 0.5

(11) Polyoxyethylene sorbitan monooleate 1.0

(12) Sodium hydroxide (1% aqueous solution) 10.0

(13) 1,3-Butanediol 5.0

(14) Preservatives Appropriate amount

(15) Spices Appropriate amount

(16) Purified water Balance

KP 545 (manufactured by Shin-Etsu Chemical Co., Ltd.): acrylic siloxane copolymer resin/decamethylcyclopentasiloxane 30% solution

KF 6015 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.5)

KP 561 (manufactured by Shin-Etsu Chemical Co., Ltd.): Acrylic siloxane copolymer resin: Stearyl-modified acrylate siloxane

[Preparation]

A: Mix components (1)-(10) and heat to dissolve.

B: Components (11)-(13) and (15) are mixed and heated.

C: Add B to A and emulsify, cool, add ingredient (14) to get O/W hand cream.

The hand cream obtained as described above has excellent adhesion, glossy makeup, very excellent makeup retention, and very excellent stability over temperature and time.

Example 43: Moisturizing Cream

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 5.0

(2)Methyltris(trimethylsiloxy)silane 5.0

(3)KF 56 3.0

(4) Liquid paraffin 5.0

(5) Pentaerythritol tetrakis-2-ethylhexanoate 3.0

(6) Cetyl 2-ethylhexanoate 5.0

(7)KF 6017 1.0

(8)KMP 594 2.5

(9) アエロジル R972 2.0

(10) Zinc stearate 2.0

(11) Vitamin E acetate 3.0

(12) Macrogol 400 1.0

(13) Sodium Lactate 1.0

(14) 1,3-Butanediol 5.0

(15) Preservatives Appropriate amount

(16) Spices Appropriate amount

(17) Purified water Balance

KF 56 (manufactured by Shin-Etsu Chemical Co., Ltd.): Methylphenylpolysiloxane

KF 6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

KMP 594 (manufactured by Shin-Etsu Chemical Co., Ltd.): Spherical silicone elastomer resin powder

Aerosil R972 (manufactured by Japan Aerosil): Hydrophobic silica

[Preparation]

A: Mix ingredients (1)-(7) and (10)-(11) evenly, add ingredients (8)-(9), and disperse evenly.

B: Components (12)-(15) and (17) are added and dissolved.

C: B was slowly added to A and emulsified, then cooled, and component (16) was added to obtain a moisturizing cream.

The moisturizing cream obtained as described above has good spreadability, moist feeling, no sticky feeling, no change with temperature or time, and excellent usability and stability.

Example 44: After Shave Cream

(Element) (%)

(1)Methyltris(trimethylsiloxy)silane 30.0

(2)Tetrakis(trimethylsiloxy)silane 5.0

(3)KF 6017 2.9

(4)KF 6026 5.0

(5) Polyethylene glycol (molecular weight: 400) 5.0

(6) Sodium L-glutamate 2.0

(7) Allantoin 0.1

(8) Aloe Vera Extract Appropriate amount

(9)Ethanol 3.0

(10) Preservatives Appropriate amount

(11) Antioxidants Appropriate amount

(12) Spices Appropriate amount

(13) Purified water Balance

KF 6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

KF 6026 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene methyl siloxane polyoxypropylene oleyl methyl siloxane dimethyl siloxane copolymer (HLB=4.7)

[Preparation]

A: Mix components (1)-(4) and heat to dissolve.

B: Components (5)-(11) and (13) are mixed and heated.

C: Add B to A, emulsify, cool, add component (12), and obtain an after-shave skin cream.

The aftershave cream obtained as described above maintains a moist feeling after application and is also excellent in stability.

Example 45: Eye Wrinkle Cream

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 3.0

(2) Methyltris(trimethylsiloxy)silane 17.0

(3)KF7312 J 5.0

(4)KF 6017 2.0

(5)KF 6026 5.0

(6) Sodium chondroitin sulfate 2.0

(7) Sodium Lactate 1.0

(8) Glycerin 50.0

(9) Preservatives Appropriate amount

(10) Antioxidants Appropriate amount

(11) Spices Appropriate amount

(12) Purified water Balance

KF 7312 J (manufactured by Shin-Etsu Chemical Co., Ltd.): Silicone resin:

50% decamethylcyclopentasiloxane solution of a siloxane network compound (trimethylsiloxysilicic acid) with a [Me ₃ SiO _1/2 ]/[SiO ₂ ] ratio of 0.8

KF 6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

KF 6026 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene methyl siloxane polyoxypropylene oleyl methyl siloxane dimethyl siloxane copolymer (HLB=4.7)

[Preparation]

A: Components (1)-(5) and (10) are heated and mixed.

B: Components (6)-(9) and (12) are heated and dissolved.

C: Slowly add B to A under stirring, emulsify, cool, and add component (11) to obtain eye wrinkle-removing cream.

The eye wrinkle removing cream obtained as described above has good film retention, does not change with temperature or time, and has excellent stability.

Example 46: Eyeshadow

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 12.0

(2)Methyltris(trimethylsiloxy)silane 3.0

(3)KF 96A-6 10.0

(4)KF 6012 2.0

(5) PEG(10) lauryl ether 0.5

(6) LL treated chromium oxide** 6.2

(7) Silicone treated Ultramarine* 4.0

(8) LL treated titanium-coated mica** 6.0

(9) Sodium chloride 2.0

(10)Propylene glycol 8.0

(11) Preservatives Appropriate amount

(12) Spices Appropriate amount

(13) Purified water Balance

KF 96A-6 (manufactured by Shin-Etsu Chemical Co., Ltd.): Dimethicone with a viscosity of 6 mm ² /s

KF 6012 (manufactured by Shin-Etsu Chemical Co., Ltd.): Polyoxyethylene-polyoxypropylene-methylpolysiloxane copolymer (HLB=7.0)

*: Silicone treatment: Add 3% of methyl hydrogen polysiloxane to the powder, and then heat treat the resultant

**: LL treatment: Powder coating treatment with 5% ^Nε -lauroyl-L-lysine (Amiho-pLL manufactured by Ajinomoto Co., Ltd.)

[Preparation]

A: Mix components (1)-(5), add components (6)-(8), and disperse uniformly.

B: Components (9)-(11) and (13) were uniformly dissolved.

C: Slowly add B to A under stirring, emulsify, add component (12), and obtain an eye shadow.

The eye shadow obtained as described above has good gloss, good make-up retention, does not change with temperature or time, and is excellent in stability.

Example 47: Eyeliner

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 5.0

(2) Methyltris(trimethylsiloxy)silane 17.0

(3)KF 96A-6 5.0

(4) ホホバ oil 2.0

(5)KF 6017 1.0

(6) Silicone treated iron oxide black (Note) 20.0

(7)Ethanol 5.0

(8) Preservatives Appropriate amount

(9) Purified water Balance

KF 96A-6 (manufactured by Shin-Etsu Chemical Co., Ltd.): Dimethicone with a viscosity of 6 mm ² /s

KF 6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

(Note) Siloxane-treated iron oxide black: Added 2% of methyl hydrogen polysiloxane to iron oxide black, followed by heat treatment.

[Preparation]

A: Heat and mix ingredients (1)-(5), add ingredient (6), and disperse evenly.

B: Components (7)-(9) are dissolved by heating.

C: Slowly add B to A under stirring, and emulsify to obtain eyeliner.

The eyeliner obtained as described above has good gloss, good make-up retention, is not easy to damage the makeup, does not change with temperature or time, and has excellent stability.

Example 48: Eyeliner

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 32.0

(2)KF 96A-6 5.0

(3) Silicone treated iron oxide black 20.0

(4) Vitamin E acetate 0.2

(5) ホホバ oil 2.0

(6) Bentonite 3.0

(7)KF 6012 2.0

(8)Ethanol 10.0

(9) 1,3-Butanediol 10.0

(10) Preservatives Appropriate amount

(11) Spices Appropriate amount

(12) Purified water Balance

KF 96A-6 (manufactured by Shin-Etsu Chemical Co., Ltd.): Dimethicone with a viscosity of 6 mm ² /s

KF 6012 (manufactured by Shin-Etsu Chemical Co., Ltd.): Polyoxyethylene-polyoxypropylene-methylpolysiloxane copolymer (HLB=7.0)

[Preparation]

A: Mix components (1)-(2), (4)-(7), add component (3), and mix and disperse evenly.

B: Ingredients (8)-(10) and (12) are mixed.

C: Slowly add B to A, emulsify, then cool, add component (11), and obtain an eyeliner.

The eyeliner obtained as described above has good gloss, good make-up retention, is not easy to damage the makeup, does not change with temperature or time, and has excellent stability.

Example 49: Antiperspirant

(Element) (%)

(1)Methyltris(trimethylsiloxy)silane 26.0

(2)Tetrakis(trimethylsiloxy)silane 4.0

(3)KF 6026 1.0

(4) Polyoxyethylene sorbitan monooleate (20E.O.) 0.5

(5) Glycinate salt of aluminum zirconium tetrachlorododecahydroxy hydrate 20.0

(6) Purified water Balance

KF 6026 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene methyl siloxane polyoxypropylene oleyl methyl siloxane dimethyl siloxane copolymer (HLB=4.7)

[Preparation]

A: Mix ingredients (1) and (2).

B: Component (4) is dissolved in (5), and component (3) is added.

C: Slowly add B to A under stirring to emulsify to obtain an antiperspirant.

The antiperspirant thus obtained has good spreadability, is not sticky, does not turn white so much, has a refreshing feeling of use, does not change with temperature or time, and is also excellent in stability.

Example 50: Antiperspirant

(Element) (%)

(1) KSG-21 20.0

(2) KSG-15 20.0

(3)Tetrakis(trimethylsiloxy)silane 10.0

(4)Methyltris(trimethylsiloxy)silane 20.0

(5) Coordination compound of aluminum zirconium tetrachlorododecahydroxy hydrate and glycine 20.0

(6)KF 96A-6 10.0

KSG-21 (manufactured by Shin-Etsu Chemical Co., Ltd.): Cross-linked polyether-modified methylpolysiloxane/dimethylpolysiloxane

KSG 15 (manufactured by Shin-Etsu Chemical Co., Ltd.): Cross-linked polyether-modified methylpolysiloxane/decamethylcyclopentasiloxane

KF 96A-6 (manufactured by Shin-Etsu Chemical Co., Ltd.): Dimethicone with a viscosity of 6 mm ² /s

[Preparation]

A: Components (1)-(4) and component (6) are uniformly mixed.

B: Add component (5) to A, mix and disperse.

The antiperspirant obtained as described above is not sticky and is very stable against changes in temperature or time.

Example 51: Transparent Gel Cosmetics

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 10.0

(2)KF 615A 10.0

(3) 1,3-Butanediol 10.0

(4) Polyethylene glycol 400 9.0

(5) 2-hydroxyoctanoic acid 1.0

(6) Sorbitol (70% aqueous solution) 10.0

(7) Citric acid Appropriate amount

(8) Sodium citrate Appropriate amount

(9) Preservatives Appropriate amount

(10) Spices Appropriate amount

(11) Purified water Balance

KF 615A (manufactured by Shin-Etsu Chemical Co., Ltd.): Polyoxyethylene-polyoxypropylene-methylpolysiloxane copolymer (HLB=14.0)

[Preparation]

A: Components (3)-(11) are uniformly dissolved.

B: Components (1)-(2) are mixed and made uniform.

C: Slowly add A to B under stirring to emulsify to obtain a transparent gel cosmetic.

The transparent gel cosmetic obtained as described above is easy to be compatible with the skin, does not change with temperature or time, and has excellent stability.

Example 52: Emulsion

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 13.0

(2)KF 96A-6 6.0

(3) Squalane 5.0

(4) Neopentyl glycol dioctanoate 3.0

(5) α-monooleyl glyceryl ether 1.0

(6)KF 6017 2.0

(7) Aluminum distearate 0.2

(8) Magnesium sulfate 0.7

(9) Glycerin 5.0

(10) Preservatives Appropriate amount

(11) Spices Appropriate amount

(12) Purified water Balance

KF 96A-6 (manufactured by Shin-Etsu Chemical Co., Ltd.): Dimethicone with a viscosity of 6 mm ² /s

KF 6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

(Preparation)

A: The ingredients (1)-(7) are heated and mixed.

B: Components (8)-(10) and (12) are heated and dissolved.

C: Slowly add B to A under stirring, emulsify, cool, add component (11), and obtain an emulsion.

The emulsion obtained as described above has low viscosity, fine texture, good spreadability, moderate moist or soft feeling, very good make-up retention, does not change with temperature or time, and has excellent stability.

Example 53: Emulsion

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 11.0

(2)Methyltris(trimethylsiloxy)silane 4.0

(3)KF 96A-6 6.0

(4) Squalane 5.0

(5) Neopentyl glycol dicaprylate 3.0

(6) α-Monooleyl glyceryl ether 1.0

(7)KF 6026 1.5

(8)KF 6017 1.0

(9) Aluminum distearate 0.2

(10) Dextrin fatty acid ester 1.0

(11)Magnesium sulfate 0.7

(12) Glycerin 5.0

(13) Preservatives Appropriate amount

(14) Spices Appropriate amount

(14) Purified water Balance

KF 96A-6 (manufactured by Shin-Etsu Chemical Co., Ltd.): Dimethicone with a viscosity of 6 mm ² /s

KF 6026 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene methyl siloxane polyoxypropylene oleyl methyl siloxane dimethyl siloxane copolymer (HLB=4.7)

KF 6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

[Preparation]

A: Ingredients (1)-(10) are heated and mixed.

B: Components (11)-(13) and (15) are heated and dissolved.

C: Slowly add B to A under stirring, emulsify, cool, add component (14), and obtain an emulsion.

The emulsion thus obtained has a refreshing feeling in use, does not change with temperature or time, and is also excellent in stability.

Example 54: Emulsion

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 10.0

(2)KF 56 5.0

(3) Squalane 5.0

(4) Pentaerythritol tetrakis-2-ethylhexanoate 5.0

(5)KF 6017 3.0

(6)KMP 594 2.0

(7) アェロジル R972 0.5

(8) Magnesium Ascorbyl Phosphate 1.0

(9) Sodium chloride 1.0

(10) Polyethylene glycol 11000 1.0

(11) Propylene glycol 8.0

(12) Preservatives Appropriate amount

(13) Spices Appropriate amount

(14) Purified water Balance

KF 56 (manufactured by Shin-Etsu Chemical Co., Ltd.): Methylphenylpolysiloxane

KF 6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

KMP 594 (manufactured by Shin-Etsu Chemical Co., Ltd.): Spherical silicone elastomer resin powder

Acerosil R972 (manufactured by Aerosil Corporation of Japan): Hydrophobic silica

[Preparation]

A: Mix ingredients (1)-(4) evenly, add ingredients (5)-(6) and disperse evenly.

B: Components (7)-(9) are added to component (13) and dissolved, and components (10) and (11) are made uniform, and then added.

C: B is slowly added to A and emulsified, then cooled, and component (12) is added to obtain an emulsion.

The emulsion obtained as described above has good spreadability, no sticky feeling, has a soft application feeling, does not change with temperature or time, and has very excellent stability.

Example 55: Beauty Essence

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 12.0

(2) Glyceryl triethylhexanoate 10.0

(3)KF 6017 2.0

(4)KSG 21 0.2

(5) Glycerin 10.0

(6) Magnesium Ascorbyl Phosphate 3.0

(7) Sodium chloride 2.0

(8) Preservatives Appropriate amount

(9) Spices Appropriate amount

(10) Purified water Balance

KF 6017 (manufactured by Shin-Etsu Chemical Co., Ltd.): polyoxyethylene-methylpolysiloxane copolymer (HLB=4.6)

KSG 21 (manufactured by Shin-Etsu Chemical Co., Ltd.): Cross-linked polyether-modified methylpolysiloxane/dimethylpolysiloxane

(Preparation)

A: The ingredients (1)-(4) are heated and mixed.

B: Components (5)-(8) and (10) are heated and dissolved uniformly.

C: Slowly add B to A under stirring, emulsify, cool, add component (9), and obtain a beauty serum.

The cosmetic liquid obtained as described above has a good affinity with the skin, and is also excellent in stability without changing with temperature or time.

Example 56: Deodorant

(Element) (%)

(1)Tetrakis(trimethylsiloxy)silane 3.0

(2)KF 96A-6 4.0

(3)KF 615A 1.0

(4) Propylene glycol 31.0

(5) Triclosan 0.1

(6) Glycerin 15.0

(7) Preservatives Appropriate amount

(8) Spices Appropriate amount

(9) Purified water Balance

KF 96A-6 (manufactured by Shin-Etsu Chemical Co., Ltd.): Dimethicone with a viscosity of 6 mm ² /s

KF 615A (manufactured by Shin-Etsu Chemical Co., Ltd.): Polyoxyethylene-polyoxypropylene-methylpolysiloxane copolymer (HLB=14.0)

[Preparation]

A: Mix ingredients (1)-(3).

B: Component (5) is dissolved in component (4), and components (6)-(9) are mixed.

C: While vigorously stirring A, add B to emulsify.

D: Add 65 parts of C and 35 parts of propellant (a mixture of n-butane, isobutane and propane) into an aerosol can to obtain a deodorant.

The deodorant obtained as described above is not sticky and has excellent stability.

Example 57: Aerosol Composition (Astringent, Deodorant)

(Element) (%)

(1) Silicone treated mica 3.0

(2) Allantoin Aluminum Chlorhydrazine 2.0

(3) Isopropylmethylphenol 0.3

(4) Sorbitan Sesquioleate 0.2

(5) Isopropyl myristate 5.0

(6)Tetrakis(trimethylsiloxy)silane 5.0

(7)Methyltris(trimethylsiloxy)silane 1.0

(8) Spices Appropriate amount

(9) Propellant Surplus

[Preparation]

A: Mix ingredients (1)-(8).

D: Fill A into an aerosol can, then fill with ingredient (9).

The aerosol composition of the present invention obtained as described above has a high deodorant effect, is not sticky when applied, and has good redispersibility, so it is very excellent in usability.

Industrial applicability

As described in detail above, tetrakis(trimethylsiloxy)silane imparts moderate volatility to cosmetics, has excellent pigment dispersibility and emulsification stability, and is suitable for use in cosmetics. In addition, the tetrakis(trimethylsiloxy)silane obtained by the method of the present invention has high purity and is suitable for mixing in cosmetics.

Claims (22)

1. cosmetics is characterized in that: contain four (trimethylsiloxy group) shown in the formula (1) silane:

[(CH ₃) ₃SiO] ₄Si (1)。

2. the cosmetics of claim 1 is characterized in that: contain the silane of methyl three (trimethylsiloxy group) shown in the formula (2):

[(CH ₃) ₃SiO] ₃SiCH ₃ (2)。

3. claim 1 or 2 cosmetics is characterized in that: further contain the volatile solvent under 1 atmospheric pressure, 25 ℃.

4. the cosmetics of claim 3, wherein above-mentioned volatile solvent are to be selected from hydrocarbon at least a that the silicon atom number is 4 or 5 straight chain shape dimethyl polysiloxane, the silicon atom number is 4-6 cyclic dimethyl polysiloxane, the pure and mild carbon number of 1 valency that carbon number is 1-3 are 10-16.

5. the cosmetics of claim 4 is characterized in that: above-mentioned volatile solvent is to be selected from one or more of octamethyltrisiloxane, decamethyl tetrasiloxane, octamethylcy-clotetrasiloxane, decamethylcyclopentaandoxane, ten diformazan basic rings, six siloxanes, ethanol, isopropyl alcohol, propanol, Fancol ID, isodecane, 2-Methylpentadecane, isoparaffin.

6. each cosmetics among the claim 1-5, these cosmetics further contain emulsifying agent, are the emulsified make-ups of w/o type.

7. the cosmetics of claim 6, wherein mentioned emulsifier be selected from polyether-modified organopolysiloxane, alkyl polyoxyalkylene altogether modified siloxane, fluoridize dimethyl polysiloxane alcohol, perfluoroalkyl polyoxyalkylene altogether modified siloxane, perfluoro alkoxy polyoxyalkylene altogether modified siloxane, glyceryl modified siloxane, polyglyceryl modified siloxane, perfluoroalkyl polyglyceryl altogether modified siloxane, and the glycosyl modified siloxane is at least a.

8. each cosmetics among the claim 1-5, it is surfactant that these cosmetics further contain nonionic, it is cleaning agent.

9. the cosmetics of claim 8, wherein above-mentioned nonionic be surfactant be selected from polyether-modified organopolysiloxane, alkyl polyoxyalkylene altogether modified siloxane, fluoridize dimethyl polysiloxane alcohol, perfluoroalkyl polyoxyalkylene altogether modified siloxane, perfluoro alkoxy polyoxyalkylene altogether modified siloxane, glyceryl modified siloxane, polyglyceryl modified siloxane, perfluoroalkyl polyglyceryl altogether modified siloxane, and the glycosyl modified siloxane is at least a.

10. each cosmetics among the claim 1-5, these cosmetics further contain methyl phenyl silicone, and it is an abluent.

11. each cosmetics among the claim 1-5, these cosmetics further contain pigment.

12. the cosmetics of claim 11, these cosmetics further contain polybutene, and it is an oil-based cosmetic preparation.

13. the cosmetics of claim 11, these cosmetics further contain water, and at least a surfactant that is selected from sorbitan fatty acid ester, polyglyceryl fatty acid ester, sucrose fatty acid ester and polyose alkylether is the solid cosmetics.

14. the cosmetics of claim 13, these cosmetics further contain one or more polyol compounds that is selected from the pure and mild saccharide of multivalence.

15. each cosmetics among the claim 1-14 is characterized in that: further contain silicone resin, silicone-modified organic binder bond, fluorine modified siloxane resin or their 2 kinds or above mixture.

16. each cosmetics among the claim 1-15 is characterized in that: further contain the anti-ultraviolet composition.

17. cosmetics is characterized in that: these cosmetics contain four (trimethylsiloxy group) silane, and described four (trimethylsiloxy group) silane is by containing the method for following step (1)-(4):

(1) mix 2-10 mole hexamethyl disiloxane, 0.01-0.5 equimolar acid catalyst in 1 mole of following tetraalkoxysilane, temperature is set at 0 ℃ or above but less than 30 ℃ step;

(2) step of 1 mole of tetraalkoxysilane of adding in the system of step (1) gained;

(3) keeping temperature is 0 ℃ or above but less than 30 ℃, and interpolation 2.5-10.0 mole of water in the system of gained to step (2) in is simultaneously reacted 30 minutes-5 hours step; And

(4) 30 minutes-5 hours step of reaction under 30-100 ℃ temperature,

The hexamethyl disiloxane that tetraalkoxysilane shown in the following general formula (A) and following chemical formula (B) are had

Si(OR) ₄ (A)

R represents that carbon number is the 1 valency alkyl of 1-10,

(CH ₃) ₃SiOSi (CH ₃) ₃(B) reaction obtains.

18. the cosmetics of claim 17 is characterized in that: tetraalkoxysilane is be selected from tetramethoxy-silicane, tetraethoxysilane and tetrapropoxysilane at least a.

19. the cosmetics of claim 17 or 18 is characterized in that: in step (1), with respect to 1 mole of tetraalkoxysilane, further mixing 0.5-10 mole carbon number is the 1 valency lower alcohol of 1-6.

20. the cosmetics of claim 19 is characterized in that: 1 valency lower alcohol is to be selected from one or more of methanol, ethanol and isopropyl alcohol.

21. each cosmetics among the claim 17-20 is characterized in that: acid catalyst is to be selected from one or more of sulphuric acid, methanesulfonic acid and trifluoromethanesulfonic acid.

22. each cosmetics among the claim 1-21 is characterized in that: 1,1,1,5,5 shown in the following formula (3), 5-hexamethyl-3-trimethylsiloxy group-3-hydroxyl trisiloxanes:

[(CH ₃) ₃SiO] ₃The content of SiOH (3) accounts for 1 quality % or following of cosmetics gross mass.