JP3454387B2 - Emulsion manufacturing method - Google Patents

Description

Detailed Description of the Invention

[0001]

FIELD OF THE INVENTION The present invention relates to a method for producing an emulsion. The present invention avoids oxidization / decomposition that occurs in the high temperature dissolution treatment step of the oil phase component when producing an emulsion, especially from the oil phase component and the water phase component, and is a heat-labile additive component such as a vitamin preparation. To avoid the deterioration of the raw materials and to oxidize, decompose and
The present invention relates to a manufacturing method for providing an excellent quality emulsion contained in a product without being affected by alteration or the like.

[0002]

2. Description of the Related Art Emulsions have been generally used in basic cosmetics and the like. Since such an emulsion is a kind of emulsion in which one of two liquids, such as water and oil, which do not dissolve in each other as a dispersed phase, is dispersed in the other dispersion medium in a stable state, various components are blended. It has the advantage that it can be done. In addition, it can be mixed with fat, moisturizer and water, so as to maintain the moisture balance of the skin, as a cosmetic suitable mainly for replenishing water, moisturizer, and fat, as well as moisturizing and softening the skin Various types of cosmetics suitable for imparting a function of being made are manufactured. Emulsion is a cosmetic product composed of an emulsion having a relatively small amount of oil and fluidity.Because of its large amount of water, it is used as a cosmetic product more suitable for maintaining the moisture balance of the skin.
It is mainly used as a cosmetic that supplements water and moisturizers, and also oil, and has a moisturizing and softening function of the skin, and has a role of maintaining and restoring the homeostatic function of the skin and other functions. . Emulsions are easy to use and easy to apply uniformly, and as described above, it is possible to mix an aqueous component and an oil-soluble component, so that, for example, a refreshing, moist, and fresh form in terms of usability. Those that spread well, those that fit quickly on the skin,
It can be made to have a variety of properties, such as one that can be easily wiped off with your hands or one that can be washed with water, and it may be different depending on the occasion, especially in the summer season, the age of the user, and the living environment. It is a convenient and useful dosage form that can be easily manufactured according to the purpose of use according to the difference in quality, condition, makeup habit, and preference. Thus, the emulsion which can be used for various purposes is important for fulfilling the original beauty of the cosmetics, which is the original purpose of cosmetics, and the role of making the beauty last longer.

At present, with the progress of understanding of the living body, the importance of its physiological function has been recognized in understanding the role of the skin and the like. The skin acts as a buffer so that mechanical action from the outside does not directly reach the inside of the body, and also acts to protect the human body from chemical irritation and action. The skin is responsible not only for such a protective effect, but also for temperature regulation and various other functions. It has been found that beautiful skin has a well-balanced function and action as described above, a proper balance between water and fat, is fresh, and is glossy. In this way, as one of the properties that milky lotion, which is one of the cosmetics for keeping the skin more beautiful, has to be outside the stratum corneum of the skin, and although it is an extremely thin film,
You can learn the function of the sebum membrane, which has various roles such as regulation of water content in the stratum corneum, protection from external stimulation or attack, and wrapping dirt.
It has come to be recognized that it is important to make things that help its work. By the way, as sebum in this sebum film, squalene, cholesterol ester, cholesterol, wax, triglyceride,
It has been found that it contains diglyceride, monoglyceride, fatty acid, etc., but in addition to this, there are also lipoproteins, polypeptides, lipopolysaccharides, sphingolipids, glycerides, phospholipids etc. It has been found.

In addition, the property of the emulsion is to prevent hyperkeratosis of the skin and to help the sebum membrane covering the stratum corneum to keep the skin fresh. There is. As an emulsion having such a function, it is necessary to supplement a substance similar to the natural moisturizing factor (NMF = Natural Moisture Factor) in the skin, or to prevent the NMF from flowing out and disappearing. It is also required to replenish various substances or to provide substances that assist their work. By the way, glycolipids, phospholipids, amino acids and the like have been known as NMF, and among them, particularly important components are amino acids, pyrrolidonecarboxylic acid (P
CA), lactate, urea, glucosamine, creatine, citric acid, organic acids, peptides, sodium, potassium, calcium, magnesium, etc., which together with keratin in the stratum corneum of the skin contribute to water retention. It is said that The milky lotion that is required to have such a function and action may be one in which squalene, cholesterol ester, cholesterol, wax, triglyceride, diglyceride, monoglyceride, fatty acid and other sebum components are added as its components, or Those having very similar properties are used, and in the production thereof, the oil phase component and the water phase component are emulsified and produced.

By the way, in this emulsification treatment, both the water phase component and the oil phase component must be uniformly dissolved. Each of the ingredients must be heat-dissolved so that they can be mixed or dissolved uniformly. And as described above, in order to impart the required function and action, the water phase and the oil phase must have a certain amount of a specific component, but at the same time, such a component must be emulsified with each other without heat treatment. It cannot be dissolved and mixed uniformly so that it can be used for processing. In particular, what is used as the oil phase component is a solid component at room temperature and must be heated to a high temperature or heated for a long time in order to uniformly mix or dissolve them. In this way, the heating and dissolution treatment step cannot be omitted, but some of the components are oxidized or decomposed when they are heated to a high temperature or heated for a long time, and they change to their original properties. Or the desired function is lost,
Furthermore, there is a problem that it turns into a harmful substance. In addition, since the emulsion has a large ratio of the amount of the aqueous component to the amount of the oily component, it has the characteristics that it spreads well on the skin as described above and is easy to fit in. It gives a feeling and is suitable for use in summer and cosmetics for normal to oily skin. However, the emulsion uses a dispersion system of water and oil that do not dissolve in each other such as water and oil with a low ratio of oily components, and in order to stabilize the emulsion system, the emulsion particles are made into fine particles, etc. In order to reduce the size of such emulsified particles, it is necessary to mix the oily components at a fairly high temperature so that they can be uniformly dissolved in each other. The impregnated oily component phase must also be emulsified with the aqueous phase, again at fairly high temperatures.
However, many of the components having desirable properties as an emulsion component are sensitive to heat, so that a component unstable to heating cannot be blended or becomes unstable after heat treatment. However, it is necessary to add an antioxidant etc. to prevent deterioration. In particular, many of those used as the oil phase component are sensitive to heat, and therefore, there is a concern that an irritant may be generated by heating or an allergic reaction may occur in the human body due to the substance generated by heating.

In the emulsion used for keeping the skin and the skin beautiful as described above, there are restrictions on the components to be added for that purpose, or unfavorable components such as antioxidants must be added. In addition, it is necessary to avoid causing allergic problems by altering some components due to the heat treatment. In particular, in the prior art, heating to 70 ° C. or higher and emulsification treatment while maintaining the temperature at 70 ° C. or higher generate irritants or, in order to suppress the formation of irritants, an antioxidant or the like is added. Must be added. Further, the additives such as the antioxidant thus added may cause further stimulants during the heat treatment at 70 ° C. or higher, or may cause a problem to the product once obtained. By the way, generally, the boiling point of a liquid is known to be able to easily lower the temperature of the boiling point by reducing the pressure of the environment surrounding the liquid, but in the case of solids, semi-solids, solid mixtures, etc. It has been theoretically pointed out that even if the pressure is reduced, a decrease in the melting temperature cannot be expected. It is considered that it is theoretically impossible to lower the melting temperature because the starting oil component as a component of the emulsion is solid.

[0007]

Means for Solving the Problems The present inventors have solved the above-mentioned problems by a simple method, avoiding the use of ingredients that are less restricted in their components and are not preferable to the skin, and use them for a long period of time. However, it is not harmful, and the skin is sensitized, and if normal emulsion is used, it is eager to develop a product that can be used with peace of mind even for users who suffer irritation and redness due to skin irritation. As a result of research and development, the present invention has been completed. That is, the present invention, in producing an emulsion from the oil phase component and the aqueous phase component, the oil phase component under reduced pressure in an inert atmosphere, and a normal
Characteristically, the mixture is dissolved and treated at a temperature lower than 30 ° C. to 59 ° C., which is lower than that in the emulsion production , and then the oil phase component and the aqueous phase component obtained by the treatment are mixed and emulsified at a low temperature. A method for producing a milky lotion is provided. Further, the present invention, from the oil phase component and the water phase component, in producing a milky lotion, the oil phase component is mixed and dissolved, and then the oil phase component and the water phase component obtained by the treatment are mixed. The present invention provides a method for producing an emulsion, characterized in that the emulsification treatment is performed at a low temperature and a reduced pressure, which are significantly lower than the conventional temperature. Furthermore, the present invention also requires that when an emulsion is produced from an oil phase component and an aqueous phase component, the oil phase component is mixed and dissolved at a low temperature under reduced pressure, and then the oil phase component thus obtained is treated. The perfume and other components are added and mixed according to the above, and the oil phase mixed component thus obtained and the aqueous phase component are mixed and emulsified under reduced pressure and low temperature, and then required for the product obtained by this treatment. Accordingly, the present invention also provides a method for producing an emulsion, which comprises mixing heat-unstable components. In the present invention as described above, the mixing and dissolving treatment step of the oil phase component is carried out at a temperature substantially lower than that in the mixing and dissolving treatment step of the oil phase component in the usual emulsion production in an inert atmosphere, but at the same time It is performed under reduced pressure. The mixing and dissolution treatment step at low temperature and reduced pressure means that the treatment is carried out at a temperature substantially lower than that in ordinary emulsion production and at a pressure low enough to achieve a substantially low temperature. This treatment step, rows <br/> is I under inert atmosphere, for example, can be carried out in a nitrogen stream. The mixing and dissolution treatment step of the oil phase components is carried out under a nitrogen atmosphere under substantially reduced pressure and substantially at a lower temperature.

In the present invention, the step of mixing and dissolving the oil phase components is carried out at 30 ° C. to 59 ° C. and under reduced pressure, preferably 35 ° C. to 58 ° C., more preferably 45 ° C. to 57 ° C. Done in. Of course, when using a raw material in which the mixing / dissolving treatment step of the oil phase component in the usual emulsion production must be carried out at a temperature of 70 ° C. or higher, the mixing / dissolving treatment step of the oil phase component is
What is necessary is that it is performed at a temperature substantially lower than that, and it does not necessarily have to be 59 ° C. or less. For example, it is performed under reduced pressure at 40 ° C. to 64 ° C., preferably 40 ° C. to 60 ° C. And more preferably 4
Performed at 5 ° C to 59 ° C, even more preferably 58 ° C
You can do the following: Further, when using a raw material in which the mixing and dissolving treatment step of the oil phase component in the usual emulsion production must be carried out at a temperature of 60 ° C. or higher, the mixing and dissolving treatment step of the oil phase component is carried out under reduced pressure. Three
Performed at 0 ° C to 55 ° C, preferably 35 ° C to 54 ° C
And more preferably at 40 ° C to 54 ° C. In the broad sense, the term "under reduced pressure" means that the pressure is lower than the normal pressure, but for example, 0 to about 300 mm.
It may be under a pressure of Hg, and a narrow range is about 0.
To about 200 mmHg, preferably about 0 to about 100 mmHg, more preferably about 0 to about 50 mmHg, and even more preferably about 0 to about 50 mmHg. 10 mmHg
Can be under pressure. It should be noted that 0 m referred to in the present invention
The mHg does not mean 0 mmHg theoretically, but means the maximum achievable degree of vacuum. In the present invention, the mixing and dissolution treatment step of the oil phase components can be performed at a temperature of 45 ° C to 58 ° C under a pressure of 0 to about 200 mmHg.

In the present invention, the emulsification treatment step can be carried out at low temperature under reduced pressure. In this case, the emulsification treatment step at a low temperature means that the emulsification treatment step is performed at a temperature substantially lower than that in the usual emulsion production. In this case, the emulsification treatment step under low temperature and reduced pressure may mean that the temperature is substantially lower than that in ordinary emulsion production, and that it is performed in a low-pressure atmosphere sufficient to achieve a substantially lower temperature. . In addition, this processing step can be performed under an inert atmosphere, for example, in a nitrogen stream.
This emulsification treatment step can be carried out under a nitrogen atmosphere under substantially reduced pressure, and it is preferably carried out substantially at a lower temperature. In the emulsification treatment step, the oil phase component can be gradually added to the agitated water phase component, or the oil phase component can be agitated and gradually added to the water phase component. This treatment step can be performed under an inert atmosphere, for example, in a nitrogen stream.
The reduced pressure of the emulsification treatment step under low temperature reduced pressure refers to an atmosphere lower than the normal pressure in a broad sense,
For example, it may be under a pressure of about 0 to about 200 mmHg, and as a narrow range may be under a pressure of 0 to 100 mmHg, preferably 0 to 50 mmHg, and more preferably 0 to 20 mmHg.
May be under pressure, even more preferably from 0 to 1
It can be under a pressure of 0 mmHg. In the present invention, the emulsification treatment step can be carried out at 45 ° C to 58 ° C under a pressure of about 0 to 200 mmHg. In the present invention, the low temperature in the emulsification treatment step at a low temperature means 30 ° C.
To 59 ° C, preferably 35 ° C to 58 ° C
And more preferably 45 ° C to 57 ° C. Of course, in the case of using a raw material that must be carried out at a temperature of 70 ° C. or higher in the emulsification treatment step in ordinary emulsion production, it may be carried out at a temperature substantially lower than that. The temperature does not necessarily have to be 59 ° C. or lower, and for example, it can be carried out under reduced pressure at 40 ° C. to 64 ° C., but it is preferably carried out at a lower temperature. The emulsification treatment step at a low temperature can be carried out at 40 ° C to 59 ° C, but it is preferably carried out at a lower temperature. Preferably 40 ° C to 58 ° C
And more preferably at 57 ° C. or lower. Further, when using a raw material for which the emulsification treatment step in the usual emulsion production must be performed at a temperature of 60 ° C. or higher, the emulsification treatment step at a low temperature is
C. to 57.degree. C., preferably 35.degree. C. to 56.degree. C., more preferably 40.degree. C. to 55.degree. Further, in the present invention, it is preferable that the mixing and dissolution treatment step of the oil phase components is continuously performed at a low temperature from the end of the emulsification treatment step. In this case, the treatment step at a low temperature means that the treatment step is performed at a temperature substantially lower than that in the usual emulsion production, and these treatment steps are performed at a low temperature and a reduced pressure. In this case, the treatment step under low temperature and reduced pressure may mean that the treatment is performed at a temperature substantially lower than that in the usual emulsion production, and an atmospheric pressure sufficient to achieve a substantially low temperature. . In the present invention, these processing steps are consistently performed at a pressure of 0 to 400 mmHg at 45 ° C to 58 ° C.
Can be done at.

In the present invention, the emulsification step is carried out under reduced pressure at 30 ° C. to 59 ° C., preferably 0 to 300.
mmHg at 45 to 58 ° C., more preferably 40 to 55 ° C. under a pressure of 0 to 200 mmHg.
C., even more preferably 0 to 50 mmHg
Can be carried out at even lower temperatures. In the present invention, the emulsification treatment step is performed by, for example, a homomixer. In the present invention, a preliminary emulsification treatment step may be provided before the emulsification step, and the preliminary emulsification treatment step can be performed in the same manner as in ordinary emulsion production, but can also be performed at a low temperature. In this case, the low-temperature pre-emulsification process step means that the pre-emulsification process is performed at a temperature substantially lower than in the usual emulsion production, and the substantially low temperature is performed, for example, under reduced pressure. It may mean something. In the pre-emulsification process, the oil phase component can be added to the gradually stirred water phase component, and conversely, the water phase component can be gradually added to the slowly stirred oil phase component. You can This treatment step can be performed under an inert atmosphere, for example, in a nitrogen stream. This pre-emulsification step is carried out under a pressure of 0 to 500 mmHg, preferably 0 to 3
It can be carried out under a pressure of 00 mmHg, more preferably under a pressure of 0 to 200 mmHg, and even more preferably under a pressure of 0 to 100 mmHg. In particular, it may be about 0 to about 10 mmHg.

In the present invention, the pre-emulsification step is
It is carried out at 30 ° C to 59 ° C, preferably 35 ° C to 58 ° C.
It can be performed at a temperature of 45 ° C, more preferably 45 ° C to 57 ° C. Of course, in the case of using a raw material in which the pre-emulsification treatment step in the usual emulsion production must be performed at a temperature of 70 ° C. or higher, if it is performed at a temperature substantially lower than that, Well, it does not necessarily have to be 59 ° C. or lower, and for example, it can be carried out under reduced pressure at 40 ° C. to 64 ° C., but it is preferably carried out at a lower temperature. The pre-emulsification step at a low temperature is performed at 40 ° C to 59 ° C, preferably 40 ° C to 58 ° C, and more preferably 57 ° C or less. When a raw material is used in which the pre-emulsification step in the usual emulsion production must be carried out at a temperature of 60 ° C or higher, the pre-emulsification step at a low temperature is carried out at 30 ° C to 57 ° C. It is carried out preferably at 35 ° C to 56 ° C, more preferably at 40 ° C to 55 ° C. In the present invention, the preliminary emulsification treatment step is performed under reduced pressure at 30 ° C to 59 ° C, preferably 45 ° C to 58 ° C under 0 to 300 mmHg.
At 40 ° C. to 57 ° C. under a pressure of 0 to 100 mmHg, and even more preferably at a lower temperature under a pressure of about 0 to about 50 mmHg. In the present invention, a heat-unstable component can be added and mixed after the emulsification process, and this is preferably performed at a low temperature. In this case, the addition and mixing treatment may be carried out at a temperature substantially lower than in the usual emulsion production, and this substantially lower temperature may be carried out under reduced pressure, for example. It may also mean that the treatment is carried out at a temperature that does not adversely affect the heat-labile compounding ingredients such as humectants. This treatment step can be performed under an inert atmosphere, for example, in a nitrogen stream.

In the present invention, this blending treatment step is
It is carried out at 10 ° C to 60 ° C, preferably 20 ° C to 58 ° C.
C., more preferably 30.degree. C. to 57.degree. C., and even more preferably 35.degree. C. to 50.degree. Further, in the present invention, this mixing treatment step can be performed under normal pressure, but in some cases, can be performed under reduced pressure. The compounding process is performed under a pressure of 0 to 760 mmHg, a pressure of 0 to 500 mmHg, a pressure of 0 to 200 mmHg, and a pressure of 0 to 100 mmHg.
It can be carried out under a pressure of g. Especially about 0 to about 1
It may be 0 mmHg. In the present invention, this compounding step is carried out at 10 ° C. to 60 ° C. under normal pressure, preferably 20 ° C. to 55 ° C. under normal pressure, more preferably 30 ° C. to 50 ° C. under normal pressure, and It is preferably carried out at 35 to 45 ° C. under normal pressure. This compounding process is performed under reduced pressure at 20 ° C, especially when dealing with heat-labile substances.
Can be carried out at temperatures from 60 to 60 ° C, and from 0 to 200 mm
It is performed at 20 to 60 ° C. under Hg, preferably at 20 to 55 ° C. at 0 to 100 mmHg, more preferably at 20 to 50 ° C. under a pressure of 0 to 50 mmHg, and Preferably 0 to 10 mmHg
It can also be carried out under pressure of 20 ° C to 45 ° C.

In the present invention, a fragrance and other components can be added and mixed, if necessary, following the mixing and dissolving treatment of the oil phase components, and a surfactant, a fragrance, a preservative, a coloring agent, a moisturizing agent, and a drug. Those selected from the group consisting of can be added to and mixed with the oil phase component according to the purpose. Further, in the present invention, during the emulsification treatment or subsequent to the emulsification treatment, a fragrance and other components can be added and mixed as required, and a surfactant, a fragrance, a preservative, a coloring agent, a moisturizer, and a drug. Those selected from the group consisting of can be added and mixed according to the purpose. As described above, in the present invention, vitamins, physiologically active substances, or the like can be added for the emulsification treatment or the compounding treatment subsequent to the emulsification treatment. The vitamins or physiologically active substances include those that are relatively unstable or extremely unstable to heat among the agents that can be added below, and one of the natural moisturizers or a function similar thereto. There are also things to do. For example, glycerol, sorbitol, lactate, a substance that acts as a humectant such as pyrrolidonecarboxylate to help the stratum corneum retain water, a lactic acid bacterium fermentation product, a bifidobacteria fermentation product, sophorolipid, a mitochondrial component, Yeast culture products, sophorolivid modified derivatives, Streptococcus
Hyaluronic acid obtained from Zoovidemics, Shikonin obtained from cell culture, etc.
Examples thereof include chitin obtained from crustaceans such as shrimp, chitosan, a tyrosinase inhibitor derived from mushrooms, bio γ-linolenic acid produced using a filamentous fungus Mortierella isaverina, a hydrolyzed soluble collagen, and β-cyclodextrin.

As described above, some of these vitamins or physiologically active substances can be mixed before being added in the emulsification treatment step. This mixing treatment can be performed in the same manner as in the usual emulsion production, but can also be performed at a low temperature. In this case, the mixing treatment step at a low temperature means that it is carried out at a temperature substantially lower than in the usual emulsion production, and this substantially lower temperature means that it is carried out under reduced pressure. May mean This treatment step can be performed under an inert atmosphere, for example, in a nitrogen stream. In the present invention, this mixing treatment step is performed at 10 ° C to 60 ° C, preferably 20 ° C to 59 ° C, more preferably 30 ° C to 58 ° C, and further preferably 3 ° C.
It may be performed at 5 ° C to 50 ° C. And in this invention, this mixing process step is preferably performed under reduced pressure. With this reduced pressure, the mixing process steps range from 0 to 50.
It is carried out under 0 mmHg, or under 0 to 300 mmHg, even under 0 to 200 mmHg, and especially under 0 to 100 mmHg. This mixing step is carried out under reduced pressure at 10 ° C to 55 ° C, preferably 0 to 50, especially when dealing with heat labile substances.
It is performed at 10 ° C to 50 ° C under 0 mmHg, more preferably 10 ° C to 45 at a pressure of 0 to 100 mmHg.
It is performed at ℃. In particular, it may be about 0 to about 10 mmHg.

In the present invention, the process of mixing the oil phase component with the fragrance and other components can be carried out in the same manner as in the usual emulsion production, but can also be carried out at a low temperature. In this case, the mixing treatment step of the oil phase component, the fragrance, and the other components at a low temperature means that the treatment is performed at a temperature substantially lower than that in the usual emulsion production, and this substantially low The term “under temperature” may mean, for example, that performed under reduced pressure. This treatment step can be performed under an inert atmosphere, for example, in a nitrogen stream. In the present invention, the mixing treatment step of the oil phase component with the fragrance and other components can be carried out at 30 ° C to 59 ° C, preferably 35 ° C to 55 ° C, more preferably 45 ° C to 55 ° C. It can be performed at ° C.
Of course, when using a raw material in which the mixing treatment step of the oil phase component with the fragrance and other components in the usual emulsion production must be performed at a temperature of 70 ° C. or higher, The mixing treatment step with the fragrance and other components may be carried out at a temperature substantially lower than that, and does not necessarily have to be 59 ° C. or lower, for example, 40 ° C. to 69 ° C. under reduced pressure. ℃
However, it is preferable to carry out at a lower temperature.
For example, it can be carried out at 40 ° C to 65 ° C.
C. to 60.degree. C., preferably 45.degree. C. to 59.degree. C., and even more preferably 55.degree.
Will be done below. In the case of using a raw material in which the mixing treatment step of the oil phase component with the fragrance and other components in the usual emulsion production must be performed at a temperature of 60 ° C. or higher, the low temperature oil phase component The mixing treatment step with the fragrance is performed at 30 ° C to 59 ° C, preferably 4
It is carried out at 0 ° C to 55 ° C, more preferably at 40 ° C to 50 ° C in special cases.

In the present invention, the reduced pressure in the mixing process of the oil phase component and the fragrance may be any as long as a substantially lower temperature can be achieved, for example, 0 to 500 mm.
Hg, or 0 to 400 mmHg, preferably 0 to 300 mmHg, more preferably 0 to 200 mmHg, even more preferably 0 to 100 mmHg.
It may be under a pressure of g. Especially about 0 to about 10 mmHg
May be In the pre-emulsification process, it is generally possible to perform the pre-emulsification with a paddle type stirrer,
In this preliminary emulsification treatment, it is better to use a high-speed homomixer to obtain better results. Further, in the main emulsification treatment, a better result can be obtained by using a high speed homomixer. As the emulsifying device, there is an open type, but a closed type is preferably used in order to mix air or to produce a product in an aseptic state. As an open type emulsifier,
Some have a paddle type stirrer, and some have a propeller type stirrer. Examples of the closed emulsification device include those equipped with a homomixer (high-speed stirrer).
As an emulsifying device, there is also a type in which a paddle type stirrer and a homomixer (high speed stirrer) are combined. The emulsification treatment can be carried out by using these emulsifiers with a mixer treatment, a colloid mill treatment, a homogenizer treatment and an ultrasonic treatment. With a homomixer, 1000-2000
0 rpm rotation, preferably 2000-4000 rpm
Rotation, more preferably 2500 to 3500 rpm. For example, in the pre-emulsification treatment, using a homomixer, rotation at 1000 to 20000 rpm,
The rotation is preferably performed at 2000 to 4000 rpm, more preferably 2500 to 3500 rpm. For example, the emulsification treatment is performed using a homomixer at 10
Rotation of 00 to 20000 rpm, preferably 2000 to
Rotation at 4000 rpm, more preferably 2500-35
It is performed by giving a rotation of 00 rpm.

The milky lotion obtained as described above is subjected to usual treatment to obtain a product. For example, the product obtained by the emulsification treatment may be subjected to deaeration treatment, filtration treatment, cooling treatment and the like, stored, and further filled in a container. Examples of the oil phase component used in the present invention include solid oil components, semi-solid oil components, fluid oil components and surfactants. Further, as the oil phase component of the present invention,
It may further contain one selected from the group consisting of a surfactant, a fragrance, a preservative, a coloring agent, a moisturizing agent, and a drug. Representative oil phase components of the present invention include, for example, fatty acids, higher alcohols, fatty acid esters, oils and fats, waxes, and surfactants.

Specific examples of the oil component of the oil phase component include:
Squalane, liquid paraffin, paraffin, petrolatum,
Hydrocarbons such as solid paraffin, microcrystalline wax, ceresin, olive oil, camellia oil, almond oil, cocoa butter, jojoba oil, macadamia nut oil,
Avocado oil, hydrogenated palm oil, coconut oil, castor oil, sesame oil, sunflower oil, peanut oil, evening primrose oil, oils and fats such as synthetic triglyceride, beeswax, lanolin, hydrogenated lanolin, waxes such as carnauba wax, candelilla wax, stearin Fatty acids such as acids, oleic acid, linoleic acid, isostearic acid, myristic acid, palmitic acid, palmitoleic acid, ricinoleic acid, lauric acid, behenic acid, cetanol, isocetyl alcohol, stearyl alcohol, isostearyl alcohol, behenyl alcohol, hexadecyl Higher alcohols such as alcohol, octyldodecyl alcohol, oleyl alcohol and cholesterol, cetyl isooctanoate, butyl stearate, isocetyl stearate, isopropyl isostearate, Cystine isopropyl, 2-octyldodecyl myristate, isobutyl palmitate,
Hexadecyl adipate, cetyl 2-ethylhexanoate, diisostearyl malate, ceryl 16-hydroxypalmitate, ceryl palmitate, myricyl palmitate, cetyl palmitate, isopropyl laurate, hexyl laurate, glyceryl monoricinoleate. , Decyl oleate, di-n-butyl sebacate,
Synthetic esters such as glycerol tri-2-ethylhexanoic acid ester, glycerin triester, pentaerythritol tetraester and cholesteryl ester, silicone oils such as methylpolysiloxane, dimethylpolysiloxane, methylphenylpolysiloxane and cyclomethicone, polyoxypropylene Examples include adducts. These can be used without any limitation as long as they are in accordance with the purpose and intent of the present invention. In particular, when silicone oils such as methylpolysiloxane are blended, it is difficult to carry out the dissolution treatment at a lower temperature under a slight reduced pressure condition. It is preferable to carry out mixed dissolution treatment.

Specific examples of the surfactant include glycerin monooleate, glycerin monostearate and the like, glycerol ester such as diglycerol dioleate, and triglyceryl ester such as glyceryl trioctanoate. , Trimethylol lopan ester, pentaerythritol ester, sorbitol ester, sucrose fatty acid ester and other sucrose ester, polyoxyethylene (P
OE) (20) sorbitan monolaurate, P
OE (20) sorbitan monostearate, P
OE (20) POE sorbitan fatty acid ester such as sorbitan monooleate ester, sorbitan ester such as sorbitan fatty acid ester, POE (20) cetyl alcohol ether, POE glycerol fatty acid ester such as POE glycerol triisostearate ester, POE (25) POE alkyl ethers such as cetyl alcohol ether, propylene glycol monostearate esters, POE / POP block polymers, non-ionic ones such as POE hardened castor oil ester, fatty acid soaps, anionic ones such as sodium alkylsulfate, alginic acid Sodium, starch derivatives, tragacanth gum, lecithin, phosphatidylserine, phosphatidylethanolamine, phosphatidylcholine, etc. . These can be used without any limitation as long as they are in accordance with the purpose and intent of the present invention.

Specific examples of typical combinations of oil phase components used in the present invention include those containing stearic acid, stearyl alcohol, and butyl stearate, stearic acid, stearyl alcohol, hydrogenated lanolin, squalane, and octyl. Containing dodecyl alcohol, containing cetanol, stearic acid, petrolatum, squalane, and glycerol tri-2-ethylhexanoic acid ester, solid paraffin, beeswax, petrolatum, and containing liquid paraffin, stearic acid, cetanol, petrolatum, liquid Paraffins and those containing isopropyl myristate, microcrystalline wax, solid paraffin, beeswax, petrolatum, hydrogenated lanolin, squalane, and those containing hexadecyl adipate, squas Orchid, stearic acid, behenyl alcohol, octyldodecyl alcohol, glyceryl trioctanoate, POE (20) sorbitan monostearate, sorbitan monostearate, lipophilic glyceryl monostearate, avocado oil,
Those containing methylpolysiloxane, concentrated glycerin, and 1,3-butylene glycol, squalane, behenyl alcohol, self-emulsifying glyceryl monostearate, octyldodecyl alcohol, lecithin, avocado oil, sesame oil, olive oil, and concentrated glycerin. Can be mentioned. Further, in the oil phase component, an oil-soluble fragrance, a moisturizer, an oil-soluble mucilage substance, an oil-soluble coloring agent, an oil-soluble drug, etc. may be added, as appropriate. In particular, the humectant can be preferably blended in the oil phase component. These can be used without any limitation as long as they are in accordance with the purpose and intent of the present invention.

As the fragrances, natural fragrances such as plant fragrances obtained from plants and animal fragrances obtained from the glandular sac of animals, those isolated from natural fragrances and those chemically synthesized based on them And synthetic flavors such as blended natural flavors and synthetic flavors. Specific examples of natural flavors include animal flavors such as musk, civet, catrium, and ambergris, rose oil,
Jasmine oil, neroli oil, lavender oil, ylang-ylang oil, tuberose oil, clary sage oil, clove oil, peppermint oil, geranium oil, patchouli oil, sandalwood oil, cinnamon oil, coriander oil, nutmeg oil, pepper oil, lemon oil, Examples include vegetable flavors such as orange oil, bergamot oil, opoponax oil, vetiver oil, oris oil, and oak moss oil. Specific examples of the synthetic fragrance include hydrocarbons such as monoterpenes and sesquiterpenes, alcohols such as aliphatic alcohols, monoterpene alcohols, sesquiterpene alcohols and aromatic alcohols, aliphatic aldehydes, terpene aldehydes and aromatics. Aldehydes such as aldehydes, alicyclic ketones, terpene ketones, ketones such as macrocyclic ketones,
Esters such as terpene ester and aromatic ester,
Examples include lactones such as undecalactone and those having a Schiff base such as auranium thiol.
-Citronellol, geraniol, l-linalool, d
-Linalool, linalyl acetate, limonene, damascon, damacenone, β-phenylethyl alcohol, farnesol, nonylaldehyde, rose oxide,
Benzyl alcohol, benzyl acetate, benzyl benzoate, jasmon, cis jasmon, jasmine lactone, indole, phytol, d-nerolidol, terpineol, pinene, nerol, camphene,
Cineol, geraniol ester, d-borneol, lavandulol, linalool ester, sesquiterpenes, methyl benzoate, methyl salicylate,
Methyl anthranilate, nerolidol, sclareol, eugenol, acetyleugenol, β-caryophyllene, methyl-n-amyl ketone, methylheptyl ketone, 1-menthol, menthone, isomentone,
1,8-Cineol, Menthyl Acetate, Mentofuran, Geranyl Formate, Geranyl Tigreto, Citronellyl Formate, Patchouli Alcohol, Patchurion, Patchurenone, α-Guayene, β-Prunesene, α- or β-Santalol , Santen, santenone, santenol, teresantalol, santalone, α- or β-santhalene, cinnamic aldehyde, 1-ferrandrene, pinene, α, β-pinene, n
-Decylaldehyde, sabinene, β-binene, elemol, methylheptenone, α-bergamotene, β-bisaborene, n-nonyl alcohol, nootkatone, p-cymen, decanal, α, δ-cadinene, ximole, beticerineol, α, β-vetibon , Vetiverol, vetiben, α, β, γ-iron, ebernic acid,
α, β-thujone, atranolin, chloroatranolin,
Camphor, naphthalene, 3-methylcyclopentadecanone, muscopyridine, civetone, skatole, castrin, castramine, isocastramine, vacdanol, bramannol, ambleine, terpineol, linal, lilial, methylionone, isoesuper, acetylcedrene, Examples thereof include methyl dihydro jasmonate, methyl jasmonate, cyclopentadecanolide, ethylene brassylate, galactsolid, ambroxane, and the like. Examples of these flavors include those produced by biotechnology such as ethylene brushlate, 3-methylcyclopentadecanone, cyclopentadecanone, cyclopentadecanolide, and civetone. These can be used without any limitation as long as they are in accordance with the purpose and intent of the present invention.

As the fragrance, the above-mentioned ones can be used alone, or any one of them can be selected and used in combination. The fragrance can be used in an amount sufficient to make the emulsion of the present invention acceptable to the user and to improve its usability. Usually about 0.0001 to about 10% by weight of the composition can be added. Examples of the water phase component used in the present invention include purified water such as distilled water or ion-exchanged water, or purified water mixed with a moisturizer or an alkali. The aqueous phase component may further contain one selected from the group consisting of a surfactant, a fragrance, a preservative, a coloring agent, a moisturizing agent, and a drug. Further, among the water phase components, particularly mucus substances, water-miscible organic solvents, water-soluble components,
For example, a water-soluble fragrance, a water-soluble colorant, a buffering agent, a drug and the like can be added. These can be used without any limitation as long as they are in accordance with the purpose and intent of the present invention. Examples of moisturizers include hydrophilic hygroscopic substances known as natural moisturizing factors (NMF = Natural Moisture Factor) or their derivatives. For example, glycolipids, phospholipids and amino acids are known. Of these, particularly important components include amino acids, pyrrolidonecarboxylic acid (PCA), lactate, urea, ammonia, glucosamine, creatine, citrate, organic acids, peptides, sodium, potassium, calcium, magnesium and the like. It is possible. As the moisturizer, glycerin, propylene glycol, sorbit, polyethylene glycol (PEG) 200, PEG 600, PEG 1000,
Polyethylene glycol such as PEG1500, dipropylene glycol, 1,3-butylene glycol, diglycerin, mannitol, maltitol, POE methyl glycoside, hyaluronic acid, hyaluronic acid such as sodium hyaluronate, chondroitin sulfate, collagen, elastin, pyrrolidonecarboxylic acid Particularly, sodium, amino acids, sugars, placenta extract, aloe extract, carrot extract, seaweed extract, milk extract, pearl solubilized product and the like can be mentioned.

As the moisturizing agent, the above-mentioned ones can be used alone, or any one of them can be selected and used in combination. Moisturizer,
The emulsion of the present invention can be blended in an amount sufficient to impart the functions of moisturizing and softening the skin, and thus the emulsion can be used in an amount that gives the user an excellent feeling of use.
Usually about 0.0001 to about 30% by weight of the composition can be added. Mucus substances include polysaccharides obtained from plants or microorganisms, proteins obtained from animals,
Further, semi-synthetic cellulose polymers, semi-synthetic starch polymers, semi-synthetic alginic acid polymers, polyvinyl polymers, alkylene oxide polymers and the like can be mentioned. Representative examples of mucous substances include guar gum, locust bin gum, carrageenan, galactan, gum arabic, tragacanth gum, pectin, mannan, starch, methyl cellulose, carboxymethyl cellulose, methyl hydroxypropyl cellulose, hydroxyethyl cellulose, ethyl cellulose, hydroxypropyl cellulose and the like. Cellulose derivative, carboxymethyl starch,
Starch derivatives such as methyl starch, alginic acid derivatives such as propylene glycol alginate, xanthan gum, dextran, succinoglucan, curdlan, gelatin, quince seed, sodium alginate, soagina, casein, albumin, collagen, carboxyvinyl polymer, polyacrylic acid Examples thereof include soda, polyvinyl alcohol, polyvinylpyrrolidone, polyvinyl methyl ether, polyethylene oxide and the like. As the water-miscible organic solvent, ethanol,
Examples include isopropyl alcohol, ethylene glycol, tetrahydrofuran, ethylene glycol monoethyl ether and the like.

As the colorant, organic synthetic pigments, natural pigments,
Examples include inorganic pigments. Organic synthetic pigments include azo dyes such as Yellow No. 5 (Sunset Yellow FCF), Red No. 505, Red No. 230 (Eosin YS), Red No. 1
No. 04 (phloxine B), red 218 (tetrachlorotetrabromofluorescein), red 223, orange 201, red 213 (rhodamine B) and other xanthene dyes, yellow 204 (Kirin Yellow SS), yellow Quinoline dyes such as No. 203 (Kirin Yellow WS),
Triphenylmethane dyes such as blue No. 1, green 201
No. (Alizanin Cyanine Green), Green No. 202 (Quinizarin Green SS), Anthraquinone dye such as Purple No. 201, Indigo dye such as Blue No. 2, Yellow 40
Examples thereof include nitro dyes such as No. 3, pyrene dyes such as Green No. 204, and nitroso dyes such as Green No. 401. As natural pigments, pigments obtained from plants such as carrot, orange, paprika, tomato, safflower tree, gardenia, perilla, turnip, grape, safflower, buckwheat, black oak skin, cacao bean, western red rape, purple root, beet, etc. Pigments obtained from mushrooms, yeasts, lacustrium worms, cactus worms, oak tree worms, kermes worms, sea urchins, β-carotene, β-apo-8-carotinal, capsanthin, lyropine, bixin , Crocin,
Carotenoid pigments such as canthaxanthin, shisonin, rafanine, ninocyanin, calsamine, safrole yellow, rutin, flavonoid pigments such as quercetin, flavin pigments such as lipoflavin, laccaic acid, carminic acid, quermesic acid, alizarin, shikonin, akanine, Quinone dyes such as Nikinochrome,
Examples include porphyrin dyes such as chlorophyll, diketone dyes such as curcumin, and betacyanidine dyes such as betanin.

Inorganic pigments and other functional pigments include mica, talc, kaolin, calcium carbonate, magnesium carbonate, silicic acid anhydride, aluminum oxide, barium sulfate and other extender pigments, red iron oxide, chromium oxide, iron oxide yellow, ultramarine blue. , Color pigments such as navy blue, carbon black, ultrafine particles of titanium dioxide, white pigments such as zinc oxide, titanium dioxide coated mica, fish scale foil, pearlescent pigments such as bismuth oxychloride, boron nitride, polymer resin particles, synthetic mica, Examples include photochromic pigments. Examples of the alkali include alkali metal hydroxides such as sodium hydroxide and potassium hydroxide, alkali metal carbonates such as sodium carbonate and potassium carbonate, and alkaline earth metal hydroxides such as magnesium hydroxide and calcium hydroxide. , Carbonates of alkaline earth metals such as magnesium carbonate and calcium carbonate, aliphatic amines such as triethanolamine, basic amino acids such as L-arginine, and borax. These can be used without any limitation as long as they are in accordance with the purpose and intent of the present invention. Drugs include vasodilators, antihistamines, anti-inflammatory agents, vitamins, nutritional supplements,
Examples include hormones, antiperspirants, anti-inflammatory agents, sebum suppressors, sebum secretagogues, metabolism improvers, hair root function activators, lipid peroxide suppressors, cell activators, and bactericides. These can be used without any limitation as long as they are in accordance with the purpose and intent of the present invention.

For example, typical agents include arbutin, melanin production inhibitors such as kojic acid, γ-oryzanol, bio γ-linolenic acid oil, guaiazulene, β
-Provitamin A such as carotene, vitamin A acetate, vitamin A such as vitamin A palmitate, vitamin C, vitamin C-2-phosphate, monostearyl ascorbate, vitamin C-2 such as vitamin C-2,6-dipalmitate, Vitamin B such as thiamine nitrate
_1st class, vitamin B ₂ such as riboflavin, vitamin B
₆ , vitamin B ₆ fatty acid ester, nicotinic acid, nicotinic acid amide, nicotinic acid benzyl ester, pyridoxine, pyridoxal, pyridoxamine and other vitamin B ₆ species, cyanocobalamin and other vitamin B ₁₂ species, tocopherol acetate, tocopherol calcium succinate, etc. Vitamin E and its derivatives, Cholecalciferol, Ergocalciferol and other vitamin D
, Pantothenic acid, pantothenic acid such as pantothenic acid ethyl ether, pantothenyl alcohol, biotin,
Assembly extract, cepharanthin, capsicum tincture,
Ginkgo tincture, Cantharis tincture, Aloe extract, Chamomile extract, Chlorella extract, Barley leaf extract, Ginkgo leaf extract, Apricot extract, Ibukitoranoo, Ukogi extract, Yellow oak, Yellow ream, Licorice extract, Camphor, Ginseng, Shikonin , Assemblage extract, Mulberry bark, Porphyra extract, Toki, Tomato oil, Traumatic acid, Garlic extract, Mint oil, Hinokitiol, Hechima extract, Mukuroji extract, Reishi extract, Quince mellow substance, Safflower, Waremoko, Rosemarine acid extract , Minasasanishiki extract, Erabu sea snake extract, canthali tincture, protease, lysozyme, lipase, muramidase and other enzymes, tissue respiration factor, acetylcholine, glutathione, estradiol, ethinyl estradiol and other female formo , Androgen, pituitary hormones, prostaglandins, follicle hormones such as diethylstilbestrol, beta-glycyrrhetinic acid, glycyrrhizic acid derivatives, such as dipotassium glycyrrhizinate, allantoin such as allantoin, azulene, epsilon
Corticosteroids such as aminocaproic acid, hydrocortisone, prednisone, prednisolone, chlorpheniramine maleate, diphenhydramine hydrochloride, acetylsalicylic acid, ibuprofen, oxyphenbutazone, flufenamic acid, indomethacin, sulindac, naproxen, ketoprofen, pranoprofen, piroxicam , Ε-aminocaproic acid, sulfur, urocanic acids such as urocanic acid, 3- (3,4-dihydroxyphenyl) -L-alanine, succinic acid, diisopropylaminodichloroacetate, thioxolone, urea, potassium bromate, minoxidil, zinc pyrithione, Picton olamine, chlorhexidines, halocarban and the like can be mentioned. L-, which is known as a lipid peroxide inhibitor,
Cystine, L-cysteine, or a derivative thereof,
Epicholestanol or its phosphoric acid ester, EGF, ribonucleic acid, deoxyribonucleic acid, cattle known as cell activating agents, such as superoxide dismutase (SOD), tannin, enju, rutin, pralmine, platonin, capsaicin, and yellow gon extract Examples include placenta-derived skin fibroblast activator-containing liquid, calf serum extract, bovine spleen extract, L-arginine, royal jelly and the like. In addition, those listed as humectants, those listed as vitamins or physiologically active substances, and other additives are also considered as drugs when utilizing a specific activity possessed by them, for example, biological activity.

The compounding ratio of the typical drug used in the present invention is selected in a wide range depending on the purpose and the properties of the final product obtained. For example, in the case of natural vitamin E etc., 0.001% by weight to 1.00% by weight. %, Preferably 0.0
10% to 0.50% by weight, more preferably 0.15%
The amount is from 0.3% to 0.30% by weight, but it is possible to add more than this. Further, in the case of bio γ-linolenic acid oil or the like, it is 0.05% by weight to 3.00% by weight, preferably 0.1% by weight.
It is 0% to 1.50% by weight, more preferably 0.50% to 1.00% by weight, but more than this can be added. Furthermore, guaiazulene or β-
In the case of carotene, etc., 0.00001% by weight to 1.00% by weight, preferably 0.0001% by weight to 0.2% by weight,
More preferably, it is 0.0004% by weight to 0.05% by weight, but more than this can be added. In the present invention, the product emulsion may further contain a UV control agent, a UV absorber, etc., for example, a cinnamic acid-based UV absorber, a benzoic acid-based UV absorber, a dibenzoylmethane-based agent. An ultraviolet absorber is mentioned. In the present invention, a chelating agent such as EDTA and a buffering agent such as sodium citrate, lactic acid and sodium lactate may be added to the product emulsion. Although a preservative such as paraben can be added, the addition can be omitted when the product emulsion is refrigerated or frozen. The emulsion product of the present invention that has been refrigerated or frozen may sometimes have an excellent feeling of use.

[0028]

EXAMPLES The present invention will now be described in more detail by way of examples, which are merely for better understanding of the present invention and are not intended to limit the present invention. According to the idea, various modes can be easily derived by those skilled in the art. Example 1: Component Compounding amount (a) Oil phase component (wt / wt) (1) Stearic acid 2.00 (2) Cetyl alcohol 1.50 (3) Vaseline 4.00 (4) Squalane 5.00 (5 ) Glycerol tri-2-ethylhexanoic acid 2.00 ester (6) Sorbitan monooleate 2.00 (7) Perfume 0.01 (b) Aqueous phase component (8) Purified water 73.48 (9) Triethanol Amine 1.00 (10) Dipropylene glycol 5.00 (11) PEG 1500 3.00 (c) Other components (12) Natural vitamin E 0.20 (13) Bio γ-linolenic acid oil 0.80 (14) ) Β-carotene 0.01 Total 100.00

The oil phase components (1) to (7) were combined and a "Mizuho vacuum emulsifier PVQ-5" was used. The battle mixer was about 100 rpm, and the homomixer was about 500 rpm.
While stirring at rpm under a pressure of about 20-30 mmHg,
The mixture was gradually heated and the solubility of the mixture was observed. At about 49 ° C, insoluble matter was observed in a part of the mixture, at about 51 ° C, only a slight amount of insoluble matter was observed, and at about 52 ° C, almost transparent dissolution was observed. Approximately 20 to 30 m while gradually adding the aqueous phase components (8) to (11), which have been previously subjected to dissolution treatment at 52 ° C., to the obtained dissolved product.
Under a pressure of mHg, the battle mixer is about 30 rpm, and the homomixer is about 2500 rpm with stirring at about 52 ° C. to emulsify and mix. The phase inversion occurred at about 35% of the water phase part. A liquid prepared by mixing the components (12) to (14) at room temperature in advance is brought to 40 ° C., and the emulsion thus obtained is mixed at 40 ° C., and cooled while gently stirring, and further 30 It cooled to 0 degreeC and obtained the target emulsion. The emulsified state of the product was excellent. The stability was good even after storage for 1 week under refrigeration. The emulsion was fine and uniform. The emulsion thus obtained is subjected to a sensory test by 5 panelists. The above emulsion is applied to the skin of 5 women aged 20 to 30 times twice a day in the morning and in the evening. As a result, the feeling of use was good in all cases, the emulsion was not irritated by any panelist, and the skin did not become red or itch at all.

Example 2 The dissolution treatment of the mixture of the first oil phase components (1) to (7) of Example 1 and the emulsification treatment with the addition of the water phase component were carried out under a pressure of about 100 mmHg,
The same ingredients were used and treated as in Example 1 except that the aqueous phase ingredients were mixed at about 56 ° C. Oil phase component (1) ~
In the mixture of (6), insoluble matter was observed in a part of the mixture at about 50 ° C, a slight amount of insoluble matter was observed at about 54 ° C, and at about 56 ° C, it was observed that the mixture was almost transparent. Was done.
The phase inversion occurred at about 35% of the water phase part. The emulsified state of the product was excellent. The stability was good even after storage for 1 week under refrigeration. A fine and even emulsion was obtained.

Example 3: First oil phase components (1) to (6)
The dissolution treatment of the mixture and the emulsification treatment with the addition of the water phase component are performed under a pressure of about 200 mmHg to reduce the water phase component to about 5
The same ingredients were used and treated as in Example 1 except mixing at 8 ° C. For the mixture of the oil phase components (1) to (6), an insoluble matter was observed in a part of the mixture at about 50 ° C and about 54 ° C, a slight insoluble matter was observed at about 57 ° C, and about 58 ° C.
Then, it was observed that it was almost transparently dissolved. The phase inversion occurred at about 35% of the water phase part. The emulsified state of the product was excellent. The stability was good even after storage for 1 week under refrigeration. A fine and even emulsion was obtained.

Comparative Example 1: The first mixture of the oil phase components (1) to (7) of Example 1 was dissolved under normal pressure, and the emulsification treatment with the addition of the water phase component was carried out at a pressure of about 460 mmHg. The same components as in Example 1 were used and treated in the same manner, except that the aqueous phase components were mixed at about 60 ° C. It was observed that the mixture of the oil phase components (1) to (6) was partially insoluble at about 50 ° C and about 55 ° C, and finally dissolved at about 60 ° C almost transparently. Phase inversion is about 3 in the water phase
It happened at 5%.

Example 4: Ingredient amount (A) Oil phase component (wt / wt)     (1) Squalane 2.00     (2) Stearic acid 4.00     (3) Behenyl alcohol SR 2.00     (4) 2-octyldodecanol 2.00     (5) Isopropyl palmitate 4.00     (6) Glycel tri-2-ethylhexanoate 4.00     (7) NIKKOL TS-10 0.40     (8) Kurodaran SWL 1.00     (9) KF-96 100 cps 0.40   (10) 1,3-BG 4.00   (11) Concentrated glycerin 0.40   (12) Arge colloid (2.0%) 4.00 (B) Water phase component   (13) Purified water 66.80   (14) Potassium hydroxide solution (10.0%) 1.00 (C) Other ingredients   (15) Natural Vitamin E 0.20   (16) Bio γ-linolenic acid oil 0.80   (17) β-carotene 0.01                                             Total 100.00

The oil phase components (1) to (12) are combined together,
"Mizuho vacuum emulsifier PVQ-5" is used, the battle mixer is about 100 rpm, and the homomixer is about 5
While stirring at 00 rpm, the mixture was gradually heated under a pressure of about 20 to 30 mmHg, and the solubility of the mixture was observed. About 47
An insoluble matter was observed in a part of the mixture at 0 ° C, a slight amount of insoluble matter was observed at about 49 ° C, and a substantially transparent solution was observed at about 51 ° C. About 20 to 30 while gradually adding the aqueous phase components (13) to (14), which have been previously subjected to a dissolution treatment at 51 ° C., to the obtained dissolved product.
Under a pressure of mmHg, the battle mixer is about 30 rpm, and the homomixer is about 2500 rpm with stirring at about 51 ° C. to emulsify and mix. The phase inversion occurred at about 30% of the water phase part. A liquid in which the components (15) to (17) were mixed at room temperature in advance was brought to 40 ° C., the emulsion thus obtained was mixed at 40 ° C., and the mixture was cooled while gently stirring, and further 30 It cooled to 0 degreeC and obtained the target emulsion. The emulsified state of the product was excellent. The stability was good even after storage for 1 week under refrigeration. The emulsion was fine and uniform. The emulsion thus obtained is subjected to a sensory test by 5 panelists. The above emulsion is applied to the skin of 5 women aged 20 to 30 times twice a day in the morning and in the evening. As a result, the feeling of use was good in all cases, the emulsion was not irritated by any panelist, and the skin did not become red or itch at all.

Example 5 The dissolution treatment of the first mixture of the oil phase components (1) to (12) of Example 1 and the emulsification treatment with the addition of the water phase component were carried out under a pressure of about 100 mmHg. The same ingredients were used and treated as in Example 4, except that the phase ingredients were mixed at about 53 ° C. Oil phase component (1) ~
Regarding the mixture of (12), insoluble matter was observed in a part of the mixture at about 50 ° C, and slight insoluble matter was observed at about 52 ° C.
At about 53 ° C., almost transparent dissolution was observed. The phase inversion occurred at about 30% of the water phase part. The emulsified state of the product was excellent. The stability was good even after storage for 1 week under refrigeration. A fine and even emulsion was obtained.

Comparative Example 2: The first mixture of oil phase components (1) to (12) of Example 1 was dissolved under atmospheric pressure,
The emulsification treatment with the addition of the aqueous phase component was carried out under a pressure of about 460 mmHg, and the same components as in Example 4 were used and treated except that the aqueous phase component was mixed at about 56 ° C. It was observed that the mixture of the oil phase components (1) to (12) was partially insoluble at about 50 ° C and about 52 ° C, and finally dissolved at about 56 ° C almost transparently. The phase inversion occurred at about 30% of the water phase part.

As is clear from the above Examples and Comparative Examples, it was unexpectedly clarified that the dissolution treatment can be carried out at a lower temperature by dissolving the oil phase component under reduced pressure. Generally, the melting temperature of the oil phase component varies depending on the source, natural or synthetic, and the composition of the mixed components, but it is usually at least 70 ° C. or more, and generally 80 ° C. or more because it completely dissolves. Although it has been heated and dissolved up to the above, it has been found that by heating under reduced pressure, it can be dissolved substantially at a lower temperature so that it can be practically used for producing a cosmetic emulsion. This is completely unexpected from the physicochemical theoretical prediction that unlike the boiling point, it is unlikely to lower the melting point even if the pressure is reduced, except for special things such as sublimation. The melting point of the mixture shows a behavior that it starts melting at a temperature lower than that of a pure substance and in a wider range, and completely melts. However, in view of the relationship between the melting point and the pressure, even if the pressure is reduced to 0 mmHg, it is higher than 1 ° C. The melting point should never drop. It is not known that the oil phase component mixture, which is the raw material of the cosmetic emulsion, can be dissolved at such a lower temperature by applying a reduced pressure. This is not based on theoretical or detailed observation of phenomena, but a large amount of air, etc. is contained in the solid of the oil phase component mixture, which is the raw material of the cosmetic emulsion, and these gas components expand due to heating. It is considered that, when it comes out, it acts as an adiabatic phase on the surface of a solid or the like and inhibits heat transfer, and as a result, melting cannot be achieved unless a high temperature is used in a normal melting treatment. However, it is considered that air or the like that forms an adiabatic phase can be efficiently removed from the surface of a solid or the like in a depressurized state, and the heat transfer property is not hindered. Therefore, the present invention is an embodiment including a method for achieving the dissolution treatment of the oil phase component mixture, which is a substantially milder raw material of the cosmetic emulsion, by any method based on such an idea. When the oil phase component mixture of cosmetics is heated for a long time or heated to a high temperature, some components of a complex composition are oxidized or decomposed, but the method of the present invention effectively prevents them. I will provide a.

Example 6: Ingredient amount (A) Oil phase component (wt / wt)     (1) Stearic acid 2.00     (2) Cetyl alcohol 1.50     (3) Vaseline 4.00     (4) Squalane 5.00     (5) Glycerol tri-2-ethylhexanoic acid 2.00           ester     (6) Sorbitan monooleate 2.00     (7) Fragrance 0.01 (B) Water phase component     (8) Purified water 73.48     (9) Triethanolamine 1.00   (10) Dipropylene glycol 5.00   (11) PEG 1500 3.00 (C) Other ingredients   (12) Natural Vitamin E 0.20   (13) Bio γ-linolenic acid oil 0.80   (14) β-carotene 0.01                                             Total 100.00

The oil phase components (1) to (7) were put together, mixed and dissolved while stirring in the same manner as in Examples 1 to 3, and the resulting melts were previously dissolved by heating. While gradually adding the water phase component, the mixture is stirred and emulsified in the same manner as in Examples 1 to 3. Ingredient (13) Natural vitamin E, (1
4) Bio γ-linolenic acid oil and (15) β-carotene were mixed at room temperature in advance to a liquid of 40 ° C., which was mixed with the emulsion thus obtained at 40 ° C. and gently stirred. While cooling, the mixture was further cooled to 30 ° C. to obtain the desired emulsion. The emulsified state of the product was excellent. The stability was good even after storage for 1 week under refrigeration.
The emulsion thus obtained is subjected to a sensory test by 5 panelists. The above emulsion is applied to the skin of 5 women aged 20 to 30 times twice a day in the morning and in the evening.
As a result, the feeling of use was good in all cases, the emulsion was not irritated by any panelist, and the skin did not become red or itch at all.

Example 7: Ingredient amount (A) Oil phase component (wt / wt)     (1) Cetyl alcohol 1.00     (2) Beeswax 0.50     (3) Vaseline 2.00     (4) Squalane 6.00     (5) Dimethylpolysiloxane 2.00     (6) POE monooleate 1.00     (7) Glycerol monostearate 1.00     (8) Preservative 0.01 (B) Water phase component     (9) Purified water 52.48   (10) Glycerin 4.00   (11) 1,3-butylene glycol 4.00   (12) Coloring agent 0.01 (C) Other ingredients   (13) Natural Vitamin E 0.20   (14) Bio γ-linolenic acid oil 0.80   (15) Ethanol 5.00   (16) Quinceseed extract (5% aqueous solution) 20.00                                             Total 100.00

The oil phase components (1) to (8) were put together, mixed and dissolved while stirring in the same manner as in Examples 1 to 3, and the resulting melts were previously dissolved by heating. While gradually adding the water phase component, the mixture is stirred and emulsified in the same manner as in Examples 1 to 3. Further components (15) and (16) are combined and mixed with stirring as in Examples 1-3. Component (13) natural vitamin E and (14) bio γ-linolenic acid oil were mixed at room temperature in advance to 40 ° C., and the emulsion thus obtained was added to 40 ° C.
Mix with, cool with gentle stirring, and
It cooled to 0 degreeC and obtained the target emulsion. The emulsified state of the product was excellent. The stability was good even after storage for 1 week under refrigeration.

Example 8: Ingredient amount (A) Oil phase component (wt / wt)     (1) Stearyl alcohol 0.50     (2) Hardened palm oil 3.00     (3) Liquid paraffin 35.00     (4) Sorbitan sesquioleate 1.60     (5) POE (20) oleyl alcohol ether 2.40     (6) Preservative 0.01     (7) Fragrance 0.01 (B) Water phase component     (8) Purified water 30.35     (9) Dipropylene glycol 6.00   (10) PEG 400 4.00   (11) Chelating agent 0.01 (C) Other ingredients   (12) Potassium hydroxide 0.10   (13) Natural Vitamin E 0.20   (14) Bio γ-linolenic acid oil 0.80   (15) β-carotene 0.02   (16) Carboxyvinyl polymer (1.0% aqueous solution) 16.00                                             Total 100.00

The oil phase components (1) to (7) were put together, mixed and dissolved while stirring in the same manner as in Examples 1 to 3, and the resulting melt was previously dissolved by heating. While gradually adding the water phase component, the mixture is stirred and emulsified in the same manner as in Examples 1 to 3. Further, the component (16) is combined and mixed in the same manner as in Examples 1 to 3 with stirring. Further, the aqueous solutions of component (12) are combined and mixed with stirring. Ingredients (13) Natural Vitamin E, (14) Bio γ
-Linolenic acid oil and (15) β-carotene were mixed in advance at room temperature to a liquid of 40 ° C, and the emulsion thus obtained was mixed at 40 ° C and cooled with gentle stirring. Then, it was further cooled to 30 ° C. to obtain the desired emulsion. The emulsified state of the product was excellent. The stability was good even after storage for 1 week under refrigeration.

[0044]

EFFECT OF THE INVENTION In the present invention, it is possible to avoid the problem that the oil phase component of the prior art is heated and dissolved at a temperature of at least 70 ° C. or higher and subsequently emulsified, and a usual emulsion production is carried out.
In an inert atmosphere at a lower temperature of 30 ° C to 59 ° C
In addition, since the oil phase component is subjected to dissolution treatment under reduced pressure, useful components and the like that are unstable to heat can be arbitrarily added and their decomposition can be prevented. Therefore, it is possible to suppress the production of irritants, and the use of the emulsion for a long period of time does not cause the problem of allergies causing the skin to become red or itchy. In addition, according to the method of the present invention, the quality of the product is good and the feeling of use is satisfactory even though the method is manufactured at a low temperature. In the present invention, since all production can be carried out at a low temperature, it is possible to omit adding an antioxidant or the like, and prevent problems associated with decomposition of components. The product produced by the method of the present invention can omit addition of an antioxidant and the like, and has good quality even if it is stored at a low temperature. In some cases, the emulsion has no problem in use feeling or product even if it is stored by freezing and the like, and is excellent in comfort during use.

─────────────────────────────────────────────────── --- Continuation of the front page (56) References JP-A-5-4912 (JP, A) JP-A-2-258042 (JP, A) JP-A 59-164397 (JP, A) JP-A 63- 221835 (JP, A) JP-A-54-45351 (JP, A) JP-A-58-23613 (JP, A) Practical application Sho-62-160643 (JP, U) (58) Fields investigated (Int.Cl. ⁷ , DB name) A61K ^7/ 00-7/50

Claims (26)

(57) [Claims] 1. When producing an emulsion from an oil phase component and an aqueous phase component, the oil phase component is treated under a reduced pressure in an inert atmosphere.
From 30 ° C, a lower temperature than in normal emulsion production
A method for producing an emulsion , comprising mixing and dissolving at 59 ° C. , then mixing the oil phase component and the aqueous phase component obtained by the dissolution treatment in this way, and emulsifying the mixture at a low temperature. 2. The method for producing an emulsion according to claim 1, wherein the step of mixing and dissolving the oil phase components is carried out at 0 to 300 mmHg. 3. The method for producing an emulsion according to claim 1, wherein the mixing and dissolution treatment step of the oil phase components is performed under 0 to 200 mmHg. 4. The method for producing an emulsion according to claim 1, wherein the mixing and dissolving treatment step of the oil phase components is performed under 0 to 100 mmHg. 5. The method for producing an emulsion according to claim 1, wherein the mixing and dissolving treatment step of the oil phase components is performed under 0 to 50 mmHg. 6. The method for producing an emulsion according to claim 1, wherein the mixing and dissolution treatment step of the oil phase component is performed under 0 to 10 mmHg. 7. The mixing and dissolution treatment step of the oil phase components is 45 ° C.
The method for producing an emulsion according to any one of claims 1 to 7 , wherein the method is carried out at from 55 to 55 ° C. 8. emulsification processing steps, the production method of the emulsion according to any one of claims 1 to 7, characterized in that which is performed under reduced pressure. 9. The emulsification process step is 0 to 200 mmHg.
The method according to claim 1, which is performed under
9. The method for producing an emulsion according to any one of claims 8 to 10 . 10. The emulsification treatment step is 0 to 100 mmH.
method for producing milk according to any one of claims 1 to 8, characterized in that it is intended to be performed under g. 11. The emulsification process comprises 0 to 50 mmHg.
The method according to claim 1, which is performed under
9. The method for producing an emulsion according to any one of claims 8 to 10 . 12. The emulsification treatment step is 0 to 30 mmHg.
The method according to claim 1, which is performed under
9. The method for producing an emulsion according to any one of claims 8 to 10 . 13. The emulsification process comprises about 0 to about 10 mm.
Method for producing milk according to any one of claims 1 to 8, characterized in that it is intended to be performed under hg. 14. emulsification processing steps, the production method of the emulsion according to any one of claims 1 to 13, characterized in that to be performed in an inert atmosphere. 15. emulsification processing steps, the production method of the emulsion according to any one of claims 1 to 14, characterized in that which is performed at 59 ° C. from 30 ° C.. 16. emulsification processing steps, the production method of the emulsion according to any one of claims 1 to 14, characterized in that which is performed at 55 ° C. from 45 ° C.. 17. emulsification process, the method of producing milk according to any one of claims 1 to 16, characterized in that made by the homomixer. 18. The oil phase component is at least solid oil component, the production method of the emulsion according to any one of claims 1 to 17, characterized in that those containing semi-solid oil or fluid oil. 19. The oil phase component is at least solid oil component, the production method of the emulsion according to any one of claims 1 to 17, characterized in that those containing semi-solid oil, and the flow oil. 20. The oil phase component further contains one selected from the group consisting of a surfactant, a perfume, a preservative, a coloring agent, a moisturizer, and a drug.
20. The method for producing an emulsion according to any one of 19 to 20 . 21. The aqueous phase ingredients, production method of emulsion according to any one of claims 1 to 20, characterized in that contains at least purified water. 22. The aqueous phase component contains at least purified water and a humectant, which is characterized in that
22. The method for producing an emulsion according to any one of 21 . 23. The aqueous phase component contains at least purified water and an alkali, and
23. The method for producing an emulsion according to any of 22 . 24. The aqueous phase component further contains one selected from the group consisting of a surfactant, a perfume, an antiseptic, a colorant, a moisturizer, and a drug.
25. The method for producing the emulsion according to any one of 23 to 23 . 25. A fragrance, a preservative, and a color which are heat-unstable components in the cooling step subsequent to the emulsification treatment.
Agents, humectants, and the manufacturing method of emulsion according to any one of claims 1 to 24, characterized in that the addition of even selected the from the group consisting of drugs. 26. In producing an emulsion from an oil phase component and an aqueous phase component , a conventional emulsion production is carried out in an inert atmosphere.
Lower temperature than 30 ℃ to 59 ℃, and 0 to 2
The oil phase component was mixed and dissolved at 00 mmHg, and then the oil phase component and the aqueous phase component thus obtained were mixed and emulsified at 0 to 200 mmHg. At 50 ℃, it is a component that is unstable to heat.
Selected from the group consisting of preservatives, colorants, moisturizers, and drugs
3. A method of adding and mixing ones.
5. The method for producing an emulsion according to any one of 5 above.