TW201318642A - Method for producing O/W emulsified composition - Google Patents

Abstract

Provided is a convenient, economic and excellent environmentally-adaptive method for producing an O/W emulsified composition with a fine emulsion particle diameter, by using an anionic surfactant forming an α gel in water and a higher aliphatic alcohol. The method of the present invention includes the following steps: a step of formulating an O/W emulsified portion by emulsifying an oil phase containing the following components (A) and (B), and a portion (i.e., the first aqueous phase) of the aqueous phase containing the following components (C), (D) and (E) at a temperature of 80 DEG C or higher: (A) a higher aliphatic alcohol having a carbon number of from 12 to 26; (B) an oil component; (C) an α gel anionic surfactant obtained by forming α gel with the aforesaid component (A) in water; (D) a specific alkylene oxide derivative; and (E) water; and a step of stirring and mixing the aforesaid emulsified portion, and a residual aqueous phase (i.e., the second aqueous phase) at a temperature of from 10 to 35 DEG C, and then cooling; wherein the aforesaid (D) alkylene oxide derivative is 1 to 30 mass% of the aforesaid emulsified portion.

Description

Method for producing O/W emulsified composition [Related application]

The priority of Japanese Patent Application No. 2011-232643 filed on Oct. 24, 2011, and Japanese Patent Application No. 2011-239954, filed on Nov. 1, 2011, is hereby incorporated by reference. .

The present invention relates to a method for producing an O/W emulsified composition, and more particularly to a method for producing an O/W emulsified composition having a fine emulsified particle diameter by a method which is excellent in simplicity, economy, and environmental compatibility, and the O/W emulsification The composition uses an anionic surfactant which forms α-gel in water and a higher aliphatic alcohol.

In the past, an O/W emulsified composition using an alpha gel formed from a higher alcohol and an anionic surfactant in water was used as a cosmetic composition, a pharmaceutical composition, a quasi-drug, and the like (Patent Documents 1 to 4). .

In the method of preparing such an O/W emulsified composition, an oil phase in which 80 ° C or higher in which a higher aliphatic alcohol is dissolved is added to an aqueous phase in which an anionic surfactant is dissolved at 80 ° C or higher is conventionally used. The mixture is emulsified by a homogenizer or the like, and then cooled to about 35 ° C by a cooler such as Onlator. In the case of such an O/W emulsified composition, the higher aliphatic alcohol which has been dissolved in the emulsified particles of the high-temperature oil droplets appears on the surface of the emulsified particles with a decrease in temperature due to cooling, and The anionic surfactant present in water forms an aggregate (α gel) together, and surrounds the interface of the emulsified particles, contributing to the stabilization of the O/W emulsified composition (Non-Patent Document 1).

However, as in the prior art, the method of emulsification after 80 ° C or more and then cooling is required to heat the components or use the heat exchanger, so that energy is required, resulting in more unnecessary waste. In addition, the cooling device such as Onlator requires a large amount of water to be washed after use, and the environmental burden is increased.

Therefore, it is desired to develop a method which can economically and easily produce an O/W emulsified composition without heating all the components as in the past or using a cooling device such as an Onlator.

In recent years, it has been reported that a non-ionic surfactant, a linear higher alcohol capable of forming an alpha gum in water together with the nonionic surfactant, and an oil phase of an oil component, and a part of an aqueous phase are described. Emulsification at 70 ° C or higher to prepare a high concentration O/W emulsified portion, and mixing the emulsified portion with an aqueous phase of the remaining portion of 10 to 35 ° C while stirring to produce an O/W emulsified composition ( Patent Document 5).

Since this method does not require heating all the components and can produce an O/W emulsified composition without using a cooling device such as Onlator, it is excellent in simplicity, economy, and environmental suitability.

However, Patent Document 5 does not review the case of using an anionic surfactant which can form an alpha gum in water and a higher fatty acid alcohol.

Further, after reviewing the present inventors, it has been found that when a part of an anionic surfactant which can form an alpha gel in water and a higher aliphatic alcohol, an oil component, and an aqueous phase are used to prepare a high concentration O/W emulsified portion, It is extremely rare to mix the water phase of the remaining portion of the low temperature in the emulsified portion and to cool it to obtain an O/W emulsified composition. To emulsify the O/W emulsified composition having a fine particle size.

[Previous Technical Literature] [Patent Literature]

[Patent Document 1] Japanese Patent Laid-Open Publication No. 2001-348325

[Patent Document 2] Japanese Patent Laid-Open Publication No. 2005-132808

[Patent Document 3] Japanese Patent Laid-Open Publication No. 2008-44866

[Patent Document 4] Japanese Invention Patent No. 4767352

[Patent Document 5] Japanese Patent Laid-Open Publication No. 2011-74071

[Non-patent literature]

[Non-Patent Document 1] Sister Tail, "Chemistry and Application of Interface Activity", Dainippon Books, 1995, p.159-160

The present invention has been made in view of the above-mentioned prior art, and an object thereof is to provide an anionic surfactant and a higher aliphatic alcohol which form an alpha gel in water, and are provided by a method excellent in simplicity, economy, and environmental adaptability. A finely emulsified particle size O/W emulsified composition.

The inventors of the present invention have found that when a high-concentration O/W emulsified portion is prepared by using an anionic surfactant capable of forming an alpha gel in water, a higher aliphatic alcohol, an oil component, and a part of an aqueous phase, A specific amount of an alkylene oxide derivative is used, and an aqueous phase of the remaining portion of the low temperature is mixed in the emulsified portion, and the O/W emulsified composition is prepared by cooling to obtain a fine emulsified particle size. The O/W emulsified composition, 遂 completed the present invention.

That is, the method for producing the O/W emulsified composition of the present invention comprises the steps of: containing the oil phases of the following (A) and (B), and comprising the following (C) and (D) and (E) a part of the aqueous phase (first aqueous phase), which is emulsified at a temperature of 80 ° C or higher to prepare an O/W emulsified portion: (A) a higher aliphatic alcohol having a carbon number of 12 to 26, (B) an oil component, (C) an anionic surfactant which can be formed in the above (A) in water and obtains α gel, (D) an alkylene oxide derivative represented by the following formula (1), and (E) water; a step of cooling by mixing the emulsified portion with a residual aqueous phase (second aqueous phase) of 10 to 35 ° C while stirring; wherein the (D) alkylene oxide derivative is in the aforementioned emulsified portion 1 to 30% by mass.

R ¹ O—[(AO) _m (EO) _n ]-R ² (1) (wherein AO is an oxyalkylene having a carbon number of 3 to 4, and EO is an oxyethylene group; m and n are the average addition molar number of the above oxygen alkyl group and oxygen extension ethyl group, and 1 ≦ m ≦ 70, 1 ≦ n ≦ 70. The alkyl group and oxygen are 3 to 4 carbon atoms. The total of the ethyl groups, the ratio of the oxygen alkyl group is 20 to 80% by weight, the oxygen alkyl group having 3 to 4 carbon atoms and the oxygen stretching ethyl group may be a block addition or a random addition. The R ¹ and R ² groups may be the same or different alkyl groups having 1 to 4 carbon atoms.)

Furthermore, the present invention provides a method for producing an O/W emulsified composition, characterized in that (C) an anionic surfactant is an anionic surfactant selected from the group consisting of N-mercapto sulfonate type and N-mercapto glutamate type anionic surfactant.

Furthermore, the present invention provides a method for producing an O/W emulsified composition, characterized in that in any one of the above methods, the second aqueous phase in the total amount of the O/W emulsified composition is 40 to 75% by mass. .

Further, the present invention provides a method for producing an O/W emulsified composition, characterized in that, in any of the above-described methods, (A) a fat having a carbon number of 12 to 26 with respect to (B) an oil component of 10 parts by mass. The total amount of the alcohol and the (C) anionic surfactant is 0.5 to 10 parts by mass.

According to the method of the present invention, it is not necessary to heat all the components of the intended O/W emulsified composition, and the O/W emulsified composition can be produced without using a cooling device such as Onlator, so that the simplicity, economy, and environment Excellent adaptability. Further, by including a specific amount of the alkylene oxide derivative in the first aqueous phase of the emulsified portion, an O/W emulsified composition having a fine emulsified particle diameter can be easily obtained.

The method for producing an O/W emulsified composition of the present invention is characterized in that the method for producing an O/W emulsified composition obtained by emulsifying an oil phase in an aqueous phase comprises a first step and a second step which will be described later.

(1) Step 1 (step of preparing a high concentration emulsified part):

The oil phase and a part of the aqueous phase (the first aqueous phase) are emulsified at a temperature of 80 ° C or higher to prepare an O/W emulsified portion.

(2) Step 2 (cooling step):

By the aqueous phase of the aforementioned emulsified portion with the remainder of 10 to 35 ° C (2nd water) The step of mixing while stirring is carried out.

The oil phase system includes: (A) a higher aliphatic alcohol having a carbon number of 12 to 26, and (B) an oil component.

The first aqueous phase includes (C) an anionic surfactant which is formed in water (A) and obtains an α gel, (D) an alkylene oxide derivative, and (E) water.

Further, in the method of the present invention, the emulsified portion contains the (D) alkylene oxide derivative in an amount of from 1 to 30% by mass, preferably from 3 to 25% by mass.

The emulsified particle interface of the O/W emulsified composition thus obtained was formed with an α gel. The α-gel refers to an aggregate comprising a lamellar 2 molecular film formed by a surfactant together with a higher alcohol in a state of coexistence with water.

In the past, an oil phase containing (A) a higher aliphatic alcohol and an aqueous phase containing (C) an anionic surfactant which can be formed in the above (A) in water and obtained an alpha gel are at a temperature of 80 ° C or higher. The step of emulsification and cooling is carried out to obtain an O/W emulsified composition, but energy is wasted due to heating and use of a heat exchanger, and if a cooling device such as Onlator is used, it may cause economic/environmental The problem of burden.

On the other hand, in the present invention, a part (first aqueous phase) of the aqueous phase component of the target O/W emulsified composition and an oil phase component are used to prepare at 80 ° C or higher (preferably 80 to 85 ° C). The O/W emulsified portion which was emulsified at a high concentration was slowly mixed with the emulsified portion and a residual aqueous phase component (second aqueous phase) at a low temperature of 10 to 35 ° C while stirring. Thereby, the high-temperature emulsified portion is diluted and simultaneously cooled, and the higher aliphatic alcohol dissolved in the emulsified particles of the high-temperature emulsified portion appears, and the α-glue is formed together with the anionic surfactant and water at the interface of the emulsified particles. An O/W emulsified composition was obtained. Further, if the emulsification temperature is less than 80 ° C, the emulsified portion may not be dissolved. For emulsification, agitation, etc., as long as it is suitable for the general user You can choose to use the equipment you used in the past without special equipment. The order of mixing the emulsified portion and the second aqueous phase is not particularly limited.

Therefore, according to the production method of the present invention, since it is not necessary to use a cooling device such as an Onlator during emulsification, it is not necessary to heat a large amount of the aqueous phase, so that the O/W emulsified composition can be easily produced with low energy.

Further, in the present invention, the obtained O/W emulsified composition can be obtained by making the (D) alkyl oxide derivative in the emulsified portion 1 to 30% by mass, preferably 3 to 25% by mass. The emulsified particle diameter is 10 μm or less, and can be further reduced to 5 μm or less. Whether the alkylene oxide derivative in the emulsified portion is too small or too large, an O/W emulsified composition having a fine emulsified particle diameter cannot be obtained. Further, if another aqueous solvent is used instead of the alkylene oxide derivative, a fine O/W emulsified composition cannot be obtained.

As described above, the O/W emulsified composition of the present invention is produced by merely adding a high concentration O/W emulsified portion previously prepared at 80 ° C or higher using a specific amount of alkylene oxide derivative. The O/W emulsified composition having a fine emulsified particle diameter can be obtained by the aqueous phase of the remaining portion of 10 to 35 ° C. Therefore, the conventional production steps can be greatly simplified, and the economical and environmental compatibility are also excellent.

Hereinafter, the components used in the present invention will be described.

<(A) Higher aliphatic alcohol having a carbon number of 12 to 26>

In the present invention, the higher aliphatic alcohol having a carbon number of 12 to 26 in the component (A) is a component which forms an α-gel in water with an anionic surfactant of the component (C) described later.

Further, the formation of α-gel in water can be confirmed by DSC (Differential Scanning Calorimetry). That is, the higher aliphatic alcohol and the anionic surfactant are separately dissolved or dispersed in water. In the endothermic peak obtained by the sample, the endothermic peak of the sample obtained by mixing the high-grade aliphatic alcohol and the anionic surfactant together with water to form a single peak on the higher temperature side, so that the formation of the α gel can be confirmed.

The higher aliphatic alcohol to be used in the present invention includes those generally used for external compositions such as cosmetics, pharmaceuticals, and quasi-drugs. For example, a saturated linear monohydric alcohol may, for example, be dodecyl alcohol (= lauryl alcohol), tridecyl alcohol, tetradecanol (=myristyl alcohol), pentadecyl alcohol, cetyl alcohol (=cephthyl alcohol), heptadecyl alcohol , octadecyl alcohol (=stearyl alcohol), nonadecanol, pentaerythritol (=arachyl alcohol), twenty-one alcohol, twenty-diol (= behenyl alcohol), twenty-three alcohol, two Tetradecanol (= carnaubyl alcohol), barcoal alcohol, hexadecanol (= ceryl alcohol), and the like. Examples of the unsaturated monohydric alcohol include, for example, elaidyl alcohol. From the standpoint of stability over time, a saturated linear monohydric alcohol having a carbon number of 12 to 26 (preferably having a carbon number of 18 to 22) is preferred.

(A) The higher aliphatic alcohol may be used singly or in combination of two or more kinds, and it is preferred to use a mixture of two or more kinds of higher aliphatic alcohols. From the viewpoint of temperature stability of the O/W emulsified composition, a combination in which the melting point of the mixture is 60 ° C or higher is more preferable. An example of a suitable combination is a combination of stearyl alcohol and behenyl alcohol.

(A) The higher aliphatic alcohol is desirably 18 or more in terms of an average carbon number obtained by arithmetical average of carbon numbers. When the average carbon number is less than 18, the melting point of the O/W emulsified composition becomes low, and the high temperature stability may be insufficient. Further, the upper limit of the average carbon number is not particularly limited, but it is preferably about 22 carbon atoms.

In the present invention, usually, the amount of the (A) higher aliphatic alcohol is from 0.05 to 10% by mass, preferably from 0.1 to 6% by mass, based on the total amount of the O/W emulsified composition.

<(B) oil content>

The oil system used in the present invention is not particularly limited, and is generally used for general use. For external use such as cosmetics, pharmaceuticals, and quasi-drugs. Preferred are, for example, polar oils such as hydrocarbon oils and ester oils, silicone oils, liquid fats and the like, but are not limited thereto.

The hydrocarbon oil may, for example, be liquid paraffin, squalane, squalene, paraffin, isoparaffin, ceresin or the like.

The polyoxyxene oil can be exemplified by a chain polyphosphonium such as dimethylpolysiloxane, methylphenyl polyoxyalkylene or methylhydrogenpolyoxane; octamethylcyclotetraoxane a cyclic polyfluorene oxide such as decamethylcyclopentaoxane or dodecamethylcyclohexaoxane; a polyfluorene oxide resin or a polyoxyxene rubber having a three-dimensional mesh structure.

Examples of polar oils such as ester oils include neopentyl alcohol tetraethyl hexanoate, ethyl cetyl ethyl hexanoate, jojoba oil, and lauric acid glutamic acid bis (phytosterol/octyldodecyl) ester. , triisosostearin, glyceryl diisostearate, triethylhexanoin, dimer linoleic acid (phytosterol / hawthorn) ester, dimerization Linoleic acid (phytosterol / isostear / cetyl / hard fat / hawthorn) ester, isopropyl palmitate, phytosteryl macadamiate, neopentyl alcohol four (mountain) Capric acid/benzoic acid/ethylhexanoate), ethylhexyl palmitate, myristyl myristate, tripropylene glycol bis(trimethylacetate), and the like.

Examples of the liquid fats include linseed oil, Camellia japonica oil, Hawaiian soybean oil, corn oil, mink oil, olive oil, avocado oil, sasanqua oil, castor oil, safflower oil, sunflower oil, Almond oil, rapeseed oil, sesame oil, soybean oil, peanut oil, triglycerin, tricaprylin, glyceryl triisostearate, and the like.

One or two or more kinds of oils may be used in combination.

In the present invention, the amount of the oil component is not particularly limited, and is usually 0.1 to 20% by mass, preferably 0.2 to 15% by mass based on the total amount of the O/W emulsified composition.

<(C) anionic surfactant>

In the present invention, the anionic surfactant of the component (C) and the component of the higher aliphatic alcohol of the component (A) form a component of α gel in water.

The anionic surfactant used in the present invention is generally used for external compositions such as cosmetics, pharmaceuticals, and quasi-drugs. For example, fatty acid soaps (eg, sodium laurate, sodium palmitate, etc.); higher alkyl sulfate salts (eg, sodium lauryl sulfate, potassium lauryl sulfate, etc.); alkyl ether sulfates (eg, POE- Triethanolamine lauryl sulfate, POE-sodium lauryl sulfate, etc.; N-mercaptocreatine (for example, sodium lauroyl sarcosinate, etc.); higher fatty acid decyl sulfonate (for example, N-myristyl-N-methyl taurine, coconut oil fatty acid methyl taurate, sodium lauryl methyl taurate, etc.; phosphate ester (POE-oleyl ether sodium phosphate, POE - stearyl ether phosphate, etc.; sulfosuccinate (for example, sodium di-2-ethylhexylsulfosuccinate, monolaurinyl monoethanol decylamine polyoxyethyl sulfosuccinate, lauryl Polypropylene glycol sulfosuccinate, etc.; alkylbenzene sulfonate (for example, sodium linear dodecylbenzenesulfonate, linear dodecylbenzenesulfonic acid triethanolamine, linear dodecylbenzenesulfonic acid, etc.); Acid ester sulfate (for example, hardened coconut oil fatty acid glyceride sodium sulfate, etc.); N-mercapto glutamate (for example, N-lauryl thiol glutamic acid single , N-stearyl glutamic acid disodium, N-myristyl-L-glutamic acid monosodium, etc.; POE-alkyl ether carboxylic acid; POE-alkyl allyl ether carboxylate; --olefin sulfonate; higher fatty acid ester sulfonate; secondary alcohol sulfate; higher fatty acid alkanolamine sulfate; lauryl monoethanol amide sodium succinate; N-lipid base Aspartic acid bis(triethanolamine); casein sodium and the like.

An example of a preferred anionic surfactant is a long-chain mercaptosulfonate-type anionic surfactant represented by the following formula (I).

R ₁ CO-a-(CH ₂ ) _n SO ₃ M ₁ (I)

In the formula (I), R ₁ CO- represents a saturated or unsaturated aliphatic fluorenyl group having 10 to 22 carbon atoms. R ₁ CO can be exemplified by C ₁₁ H ₂₃ CO, C ₁₂ H ₂₅ CO, C ₁₃ H ₂₇ CO, C ₁₄ H ₂₉ CO, C ₁₅ H ₃₁ CO, C ₁₆ H ₃₃ CO, C ₁₇ H ₃₅ CO, coconut fatty acid. (coconut fatty acid) residue, oil palm fatty acid residue, etc. (a fatty acid residue refers to a group obtained by removing an OH group from a carboxyl group of a fatty acid). Further, from the viewpoint of safety and the like, it is more preferable that R ₁ CO is 12 to 22 carbon atoms.

a is -O- or -NR- (except that R represents a hydrogen atom or an alkyl group having 1 to 3 carbon atoms). These are electronic supply bases. a is preferably -O-, -NH- or -N(CH ₃ )-.

M ₁ represents an alkali metal, an alkaline earth metal, an ammonium or an organic amine. M ₁ can be exemplified by, for example, lithium, potassium, sodium, calcium, magnesium, ammonium, monoethanolamine, diethanolamine, triethanolamine, sodium taurate, sodium N-methyltaurate or the like.

The n system represents an integer of 1 to 3.

In the above formula (I), a compound in which a represents -O-, that is, a long-chain mercapto 2-hydroxyethanesulfonate-type anionic surfactant, is exemplified by cocoyl 2-hydroxyethanesulfonate. An acid salt, a stearyl 2-hydroxyethanesulfonate, a lauryl 2-hydroxyethanesulfonate, a myristyl 2-hydroxyethanesulfonate or the like.

In the above formula (I), a compound in which a represents -NH-, that is, a long-chain mercapto taurate-type anionic surfactant, may be exemplified as N-lauroyl taurate, N- Cocoyl-N-ethanol taurate, N-myristyl taurate, N-stearyl sulfonate taurate, and the like.

In the above formula (I), a compound in which a represents -N(CH ₃ )-, that is, a long-chain mercaptomethyltaurate-type anionic surfactant, can be exemplified as N-lauric acid- N-methyltaurate, N-lipidinyl-N-methyltaurate, N-stearyl-N-methyltaurate, N-cocoyl-N- Methyl taurates and the like.

Among these, a long-chain mercaptomethyltaurate-type anionic surfactant is preferred, and N-stearin such as N-stearyl-N-methyltaurate is preferred. Base-N-methyltaurate.

Further, examples of other preferable anionic surfactants include long-chain mercapto glutamate type anionic surfactants represented by the following formula (II).

R ₂ CO-NH-CH(COOM ₂ )-CH ₂ CH ₂ -COOM ₂ (II)

The R ₂ CO- is a saturated or unsaturated aliphatic fluorenyl group having 16 to 22 carbon atoms. The M ₂ system represents an alkali metal, an alkaline earth metal, an ammonium or an organic amine. M ₁ may, for example, be lithium, potassium, sodium, calcium, magnesium, ammonium, monoethanolamine, diethanolamine, triethanolamine, sodium taurate or sodium N-methyltaurate.

Representative examples include, for example, N-stearyl sulfonyl-L-glutamate, N-lipidinyl-L-glutamate, N-stearyl glutamic acid-L-triethanolamine, and the like.

In the present invention, the anionic surfactant is 0.01 to 5% by mass, preferably 0.02 to 3% by mass based on the total amount of the O/W emulsified composition. The anionic surfactant may be used alone or in combination of two or more.

In the emulsified particle interface of the O/W emulsified composition obtained by the present invention, (A) the higher aliphatic alcohol and the (C) anionic surfactant form an aggregate comprising a flaky 2-molecular film, and become a so-called alpha gel. status.

Since the α-gel system contributes to the stabilization of the O/W emulsified composition, (A) higher aliphatic alcohol and (C) anionic property in the O/W emulsified composition relative to (B) oil component 10 parts by mass. The total amount of the surfactant is preferably from 0.5 to 10 parts by mass. When the amount is less than 0.5 part by mass, the amount of the α-gel is small, so that the stability of the obtained O/W emulsified composition may be insufficient. In addition, when it exceeds 10 parts by mass, since there are too many α gels, there will be It is a tendency to be unsatisfactory from the point of view of feeling.

Further, as described above, the α gum is an endothermic peak when measured by DSC, and the endothermic peak temperature can be regarded as the melting point of the α gel. Since the α-gel has a low viscosity at a temperature above the melting point, there is a possibility that the high-temperature stability of the O/W emulsified composition is affected.

Therefore, from the viewpoint of high-temperature stability of the O/W emulsified composition, the melting point of the α-gel is preferably higher, preferably 60 ° C or higher, more preferably 65 ° C or higher.

<(D)alkylene oxide derivative>

The alkylene oxide derivative of the component (D) may, for example, be represented by the following formula (1).

R ¹ O-[(AO) _m (EO) _n ]-R ² (1)

In the formula (1), AO is an oxygen-extended alkyl group having 3 to 4 carbon atoms, and specific examples thereof include an oxygen-extension propyl group, an oxygen-extension butyl group, an oxygen-isobutyl group, and an oxytrimethylene group. Oxytetramethylene and the like. Preferred are oxygen-extended propyl groups and oxygen-extended butyl groups.

In the present invention, in the total of the oxygen alkyl group having 3 to 4 carbon atoms and the oxygen stretching alkyl group, the ratio of the oxygen alkyl group is preferably 20 to 80% by mass, more preferably 30 to 70% by mass. . If the ratio of the oxygen alkyl group is too small, the effect of miniaturization is lowered; if it is too large, it is insoluble in water and difficult to use.

m is the average addition mole number of the oxygen alkyl group having 3 to 4 carbon atoms, and n is the average addition mole number of the oxygen extension ethyl group, and may be in the range of 1 to 70, preferably 2 to 60, respectively. Further, if the total of m and n is too large, it is sticky, so (m + n) is preferably 100 or less.

The order of addition of the ethylene oxide and the alkylene oxide having a carbon number of 3 to 4 is not specifically specified. Further, the oxygen-extended ethyl group and the oxygen-and-alkyl group having a carbon number of 3 to 4 may be a block-like addition or a random addition. In the case of the block form, it includes not only the two-stage block but also the block of three or more stages. Preferably, a random addition is exemplified.

R ¹ and R ² are an alkyl group having 1 to 4 carbon atoms, and examples thereof include a methyl group, an ethyl group, a n-propyl group, an isopropyl group, a n-butyl group, a second butyl group, and a third butyl group. It is preferably a methyl group or an ethyl group. When it is a hydrocarbon group of 5 or more, hydrophilicity will fall and it becomes hard to melt|dissolve in water. R ¹ and R ² may be the same or different.

The alkylene oxide derivative of the present invention can be produced by a known method. For example, it can be obtained by subjecting a halogenated alkyl group to an ether reaction in the presence of a base catalyst by addition polymerization of a compound having a hydroxyl group and an alkylene oxide having a carbon number of 3 to 4.

Preferred examples of the alkylene oxide derivative of the formula (1) include, for example, POE (14) POP (7) dimethyl ether, POE (36) POP (41) dimethyl ether, and POE ( 55) POP (28) dimethyl ether, POE (22) POP (40) dimethyl ether, POE (35) POP (40) dimethyl ether, POE (50) POP (40) dimethyl ether, POE (11) POP (9) dimethyl ether or the like, but is not limited thereto.

In the present invention, the emulsified portion is formulated with (D) an alkylene oxide derivative in an amount of from 1 to 30% by mass, preferably from 3 to 25% by mass.

As long as the (D) alkylene oxide derivative is from 1 to 30% by mass in the emulsified portion, it can be formulated in the second aqueous phase. Therefore, the amount of the alkylene oxide derivative in the O/W emulsified composition obtained by the present invention is hardly limited.

<(E)Water>

In the present invention, the water system is contained at least in the first aqueous phase for modulating the emulsified portion. The water contained in the first aqueous phase may be an amount of the emulsifiable portion, and is usually 55 to 90% by mass, preferably 60 to 85% by mass in the emulsified portion.

Further, it is preferably included in the second aqueous phase for cooling the emulsified portion.

The total amount of water of the O/W emulsified composition obtained by the present invention is not particularly limited. It is usually 40 to 95% by mass in the total amount of the O/W emulsified composition.

The first aqueous phase is preferably 25 to 50% by mass in the total amount of the O/W emulsified composition, more preferably 30 to 45% by mass. If the first aqueous phase is too small, the stabilized O/W emulsified composition may not be obtained. If the first aqueous phase is too large, the second aqueous phase of the cooled emulsified portion will be small, so that the economy is poor.

Further, the second aqueous phase is preferably 40 to 75 mass% of the total amount of the O/W emulsified composition, more preferably 45 to 70 mass%. If the second aqueous phase is less than 40% by mass, a sufficient cooling effect cannot be obtained, and relatively more cooling energy is required, so that the economy is poor. In addition, when it exceeds 75% by mass, the first aqueous phase in which the O/W emulsified portion is prepared is reduced, so that it tends to be difficult to prepare a stable O/W emulsified composition.

Further, the temperature of the second aqueous phase (the remaining aqueous phase) added to the O/W emulsified portion is preferably from 10 to 35 ° C, particularly preferably from 15 to 30 ° C. If it is less than 10 ° C, it will become too much energy to cool the second aqueous phase, and there is a tendency to be economically poor. Further, when it exceeds 35 ° C, a sufficient cooling effect cannot be obtained, and relatively more cooling energy is required, which is inferior in economy.

<Other ingredients>

In the O/W emulsified composition of the present invention, components generally used in cosmetics, pharmaceuticals, and the like may be blended in addition to the above-mentioned essential components, without impairing the effects of the present invention. The component may, for example, be described later, but is not limited thereto: 1,3-butanediol, dipropylene glycol, isoprene glycol, 1,2-pentanediol, 1,2-hexanediol, 2-methyl Aqueous solvent such as 1,3-propanol, ethyl carbitol, 1,2-butanediol, glycerin; polyethylene glycol and its mono- or di-alkyl ether, polyethylene glycol-polypropylene glycol Co-polymer and its mono- or di-alkyl ether, sorbitol, xylitol, maltitol, mucopolysaccharide, hyaluronic acid, chondroitin salfate, chitosan and other moisturizers Agent; methyl cellulose, ethyl cellulose, gum arabic, polyvinyl alcohol and other tackifiers; organic solvents such as ethanol; butyl hydroxy toluene, tocopherol, phytic acid and other antioxidants; benzoic acid, water Salicylic acid, sorbic acid, p-hydroxybenzoic acid ester (ethyl p-hydroxybenzoate, butyl p-hydroxybenzoate, etc.), antibacterial preservatives such as hexachlorophene; glycine, alanine, lysine, Amino acids such as leucine, serine, sulphate, phenylalanine, tyrosine, aspartic acid, aspartame, glutamic acid, taurine, arginine, histidine And its salts; thiol sarcosine (such as sodium lauryl sarcosinate), glutathione, citric acid, malic acid, tartaric acid, lactic acid and other organic acids and salts thereof; vitamin A and its derivatives; Vitamin B6 hydrochloride, vitamin B6 tri-palmitate, vitamin B6 dioctanoate, vitamin B2 and its derivatives, vitamin B12, vitamin B15 and its derivatives, vitamin B; ascorbic acid, ascorbyl phosphate (salt) , vitamin C such as ascorbyl di-palmitate; α-tocopherol, - vitamin E such as tocopherol, gamma-tocopherol, vitamin E acetate, vitamin E nicotinic acid ester; vitamins such as vitamin D, vitamin H, pantothenic acid, pantethine; Nicotinic acid amide, benzyl nicotinic acid, γ-oryzanol, allantoin, glycyrrhizinic acid (salt), glycyrrhetinic acid and its derivatives, hinokitiol , musizin, bisabolol, eucalyptol, thymol, inositol, saponin (saikosaponin), human Saponins, loofah saponins, sapindus saponins, etc.) Various agents such as ubiquinone ethyl ether, ethinyl estradiol, tranexamic acid, cepharanthine, placenta extract, etc.; Rumex japonicus, Sophora flavescens, Pleurotus ostreatus (Rumex japonicus) Nuphar japonicum), citrus, sage, thyme, Achillea alpina, mallow, chuanxiong, Swertia japonica, angelica, tang, birch ), Equisetum arvense, loofah, horse chestnut (marronnier), saxifrage, arnica, lily, Japanese mugwort, peony, aloe, medlar, sawara Such as natural extracts extracted with organic solvents, alcohols, polyols, water, aqueous alcohols, etc.; cation interfaces such as stearyltrimethylammonium chloride, benzalkonium chloride, and laurylamine oxide Active agent; polyoxyethylene ethyl glyceride, polyoxyethylene ethyl methacrylate copolymer, fatty acid polyoxyethylene ethyl sorbitol, polyoxyethylene ethyl ether, maltitol hydroxy fat Alkyl ethers, alkylated polysaccharides, alkyl glucosides, sucrose fatty acid esters, poly Oxygen-extended ethyl hardened castor oil glycerin and other nonionic surfactant; ethylenediaminetetraacetic acid disodium, ethylenediaminetetraacetic acid trisodium, sodium citrate, sodium polyphosphate, sodium metaphosphate, gluconic acid and other chelating agents ( Sequestrant); neutralizer such as potassium hydroxide, sodium hydroxide or triethanolamine.

Further, other anti-UV agents such as a fragrance, an exfoliating agent, a powder, a coloring material, a whitening agent, an ultraviolet absorber, and an ultraviolet ray scattering agent may be suitably blended in such a range as not to impair the stability and the like.

In the case of each component, usually, the lipophilic component is blended in the oil phase, and the hydrophilic component is blended in the first aqueous phase and/or the second aqueous phase.

The O/W emulsified composition of the present invention can be suitably used as, for example, a cosmetic, a medical Among the drugs and quasi-drugs, it can be applied to external compositions of the skin such as skin and hair. For example, it can be used for: lotion, cream, massage cream, cleansing cream, essence, body cream, etc.; hair cream, conditioner, conditioner, etc. Hair cosmetics; sunscreen lotion and other sunscreen cosmetics; cleansing (cleansing), makeup remover and other cleansing materials; foundation (foundation) and other make-up cosmetics;

(Example)

The present invention will be described in more detail below by way of specific examples, but the invention is not limited thereto. Further, unless otherwise specified, the blending amounts are expressed in mass%.

First, the test method employed in the present invention will be described.

<Emulsion particle size>

The emulsified particle diameter of the newly prepared O/W emulsified composition was observed with an electron microscope and evaluated by the following evaluation criteria.

(assessment basis)

○: No emulsified particles larger than 5 μm.

△: No emulsified particles larger than 10 μm.

×: There are emulsified particles larger than 10 μm.

<viscosity>

The viscosity of the O/W emulsified composition immediately after the preparation was measured at 30 ° C using a B-type viscometer (rotor No. 3, rotor rotation number: 12 rpm).

Test example 1

The O/W emulsified composition was prepared according to the composition of Table 1 below using a higher aliphatic alcohol and an anionic surfactant which formed α-gel in water. The manufacturing method will be described later.

<Sample 1-2 to sample 1-4 (Process a)

(1) The first aqueous phase (components 1 to 6) is heated and mixed, and dissolved at 80 to 85 °C.

(2) The oil phase (ingredients 7 to 11) was heated and mixed, and dissolved at 80 to 85 °C.

(3) The first aqueous phase and the oil phase are stirred and mixed by a homogenizer to prepare an emulsified portion.

(4) While stirring the emulsified portion with a homogenizer, the second aqueous phase (components 12 to 13) at room temperature (about 20 ° C) was mixed into the emulsified portion to obtain an O/W emulsified composition.

<sample 1-1 (manufacturing method b)>

(1) The aqueous phase (components 1 to 6 and components 12 to 13) was heated and mixed, and dissolved at 80 to 85 °C.

(2) The oil phase (ingredients 7 to 11) was heated and mixed, and dissolved at 80 to 85 °C.

(3) The aqueous phase and the oil phase were stirred and mixed by a homogenizer, emulsified, and cooled to 40 ° C by Onlator to obtain an O/W emulsified composition.

The composition of the sample 1-1 can be obtained by using the conventional method of Onlator (Process b) to obtain a composition of an O/W emulsified composition having a fine emulsified particle diameter.

In the case of the sample 1-2 and the sample 1-3, the O/W emulsified composition having the same composition as that of the sample 1-1 was prepared by a method of cooling the emulsified portion in the second aqueous phase (Production Method a).

When the (D) alkylene oxide derivative is not present in the emulsified portion as in the case of the sample 1-2, even if the (D) alkylene oxide derivative is present in the second aqueous phase for cooling, for example, An O/W emulsified composition having a fine emulsified particle size was obtained.

On the other hand, when the (D) alkylene oxide derivative is present in the emulsified portion as in the case of the sample 1-3, an O/W emulsified composition having a fine emulsified particle diameter can be obtained in the same manner as in the sample 1-1. Further, in terms of viscosity, an O/W emulsified composition similar to the sample 1-1 was obtained.

In addition, even when the (A) alkylene oxide derivative is present in the emulsified portion, the anionic surfactant which forms the α-gel as in the case of the sample 1-4 is different, similarly to the sample 1-3. An O/W emulsified composition having a fine emulsified particle size was obtained.

Test example 2

In the sample 1-3 of Table 1, the concentration of the (D) alkylene oxide derivative in the emulsified portion was changed and reviewed. The production of the O/W emulsified composition is carried out in accordance with Process a.

As shown in Table 2, the concentration of the (D) alkylene oxide derivative in the emulsified portion was too small or too large, and the emulsified particle size tends to coarsen. In addition, compared to The viscosity of the O/W emulsified composition of the same composition prepared by the conventional method, such as Onlator, is lowered.

Therefore, it is considered that the concentration of the (D) alkylene oxide derivative in the emulsified portion is preferably from 1 to 30% by mass, more preferably from 3 to 25% by mass.

Test Example 3

The O/W emulsified composition was prepared according to the composition of Table 3 below in accordance with Process A.

From the samples 3-1 to 3-3, it was found that even in the emulsified portion, the O/W emulsified composition having a fine emulsified particle diameter could not be obtained even if another aqueous solvent and an alcohol were used instead of the (D) alkylene oxide derivative.

Further, Sample 3-4 and Sample 3-5 are in an O/W emulsified composition of an anionic surfactant and a higher aliphatic alcohol which are used in the formation of α-gel in water, in the emulsification section. In the case where a salt having a viscosity stabilization effect and a cationic surfactant are known, the emulsified particle size cannot be made fine even if these components are used.

Therefore, it can be understood that in the method of preparing a high-concentration emulsified portion and mixing the water phase of the remaining portion of the low temperature (Process a), the aging effect of the emulsified particle diameter of the O/W emulsified composition is (D) The alkylene oxide derivatives are specific.

Test Example 4

Further, the (D) alkylene oxide derivative was changed and reviewed. The production of the O/W emulsified composition is carried out in accordance with Process a.

As shown in Table 4, although the alkylene oxide derivative represented by the formula (1) is obtained as a refining effect, in the total of the oxygen-extended ethyl group and the oxygen-extended alkyl group, the oxygen is extended. When the ratio of the alkyl group is small, the effect of miniaturization tends to be lowered. Further, if the above ratio becomes large, the alkylene oxide derivative becomes hardly soluble in water and is difficult to use.

Therefore, it is considered that the ratio of the oxygen-extended alkyl group in the total of the oxygen-extended ethyl group and the oxygen-extended alkyl group is preferably from 20 to 80% by mass, more preferably from 30 to 70% by mass.

Test Example 5

The O/W emulsified composition was produced in accordance with Process a using the formulation of Table 5 below. In either case, a fine O/W emulsified composition having an emulsified particle diameter of 5 μm or less can be obtained.

Example 1 Emulsion <2nd water phase>

3. Sanxianghan (xanthan gum) 0.1

<1st water phase>

<oil phase>

<Manufacturing method>

(1) The second aqueous phase (components 1 to 3) was mixed at room temperature and dissolved.

(2) The first aqueous phase (ingredients 4 to 9) was dissolved at 80 to 85 °C.

(3) The oil phase (ingredients 10 to 15) was dissolved at 80 to 85 °C.

(4) The first aqueous phase and the oil phase were stirred and mixed by a homogenizer to prepare an emulsified portion.

(5) While stirring the emulsified portion with a homogenizer, the second aqueous phase was added and mixed to obtain an O/W emulsion.

In Example 1, the concentration of the component 9 in the emulsified portion (components 4 to 15) was 5.8% by mass, and the viscosity of the obtained emulsion was 3,770 mPa. s/30 ° C, emulsified particle size is 1 To the range of 5 μm.

Example 2 Emulsion <2nd water phase>

<1st water phase>

<oil phase>

<Manufacturing method>

(1) The second aqueous phase (components 1 to 9) was mixed at room temperature and dissolved.

(2) The first aqueous phase (components 10 to 15) is dissolved at 80 to 85 °C.

(3) The oil phase (ingredients 16 to 21) was dissolved at 80 to 85 °C.

(4) The first aqueous phase and the oil phase were mixed and stirred by a homogenizer to prepare an emulsified portion.

(5) While stirring the emulsified portion with a homogenizer, the second aqueous phase was added and mixed to obtain an O/W emulsion.

In Example 2, the concentration of the component 15 in the emulsified portion (component 10 to component 21) was 2.6% by mass, and the viscosity of the obtained emulsion was 3,820 mPa. The emulsified particle size is 1 to 5 μm at s/30 °C.

Example 3 Emulsion <2nd water phase>

<1st water phase> 9. Refined water 34.0 <oil phase> <Manufacturing method>

(1) The second aqueous phase (components 1 to 8) was mixed at room temperature and dissolved.

(2) The first aqueous phase (ingredients 9 to 12) was dissolved at 80 to 85 °C.

(3) The oil phase (ingredients 13 to 21) was dissolved at 80 to 85 °C.

(4) The first aqueous phase and the oil phase were stirred and mixed by a homogenizer to prepare an emulsified portion.

(5) While stirring the emulsified portion with a homogenizer, the second aqueous phase was added and mixed to obtain an O/W emulsion.

In Example 3, the concentration of the component 12 in the emulsified portion (ingredients 9 to 21) was 6.3% by mass, and the viscosity of the obtained emulsion was 5,130 mPa. The emulsified particle diameter is in the range of 1 to 5 μm at s/30 °C.

Example 4 Emulsion <2nd water phase>

<1st water phase>

<oil phase>

<Manufacturing method>

(1) The second aqueous phase (components 1 to 9) was mixed at room temperature and dissolved.

(2) The first aqueous phase (components 10 to 14) is dissolved at 80 to 85 °C.

(3) The oil phase (ingredients 15 to 21) was dissolved at 80 to 85 °C.

(4) The first aqueous phase and the oil phase were stirred and mixed by a homogenizer to prepare an emulsified portion.

(5) While stirring the emulsified portion with a homogenizer, the second aqueous phase was added and mixed to obtain an O/W emulsion.

In Example 4, the concentration of the component 14 in the emulsified portion (components 10 to 21) was 4.4% by mass, and the viscosity of the obtained emulsion was 4,470 mPa. The emulsified particle diameter is in the range of 1 to 5 μm at s/30 °C.

Claims (4)

A method for producing an O/W emulsified composition, comprising: an oil phase comprising the following (A) and (B), and a part of an aqueous phase comprising the following (C) and (D) and (E) ( The first aqueous phase) is a step of emulsification at a temperature of 80 ° C or higher to prepare an O/W emulsified portion: (A) a higher aliphatic alcohol having a carbon number of 12 to 26, (B) an oil component, (C) and the foregoing ( A) an anionic surfactant which forms and obtains α gel in water, (D) an alkylene oxide derivative represented by the following formula (1), (E) water; and a step of cooling the remaining aqueous phase (second aqueous phase) at 10 to 35 ° C while stirring, wherein the (D) alkylene oxide derivative is 1 to 30% by mass of the emulsified portion; R ¹ O-[(AO) _m (EO) _n ]-R ² (1) (wherein AO is an alkylene group having a carbon number of 3 to 4, EO is an oxygen-extended ethyl group, and m and n are each The average addition molar number of the alkyloxy group and the oxygen-extended ethyl group, and 1 ≦ m ≦ 70, 1 ≦ n ≦ 70; the total of the oxygen-extended alkyl group and the oxygen-extended ethyl group having 3 to 4 carbon atoms, The ratio of oxygen alkyl groups is 20 to 80% by weight; the oxygen alkyl group having 3 to 4 carbon atoms and the oxygen stretching ethyl group may be block-like addition , May also be a random type adduct; R ^1, R ² may be the same or different lines of alkyl having 1 to 4). The method for producing an O/W emulsion composition according to claim 1, wherein the (C) anionic surfactant is selected from the group consisting of N-mercaptosulfonate anions. Sexual surfactant and N-mercapto glutamate type anionic surfactant. The method for producing an O/W emulsified composition according to the first or second aspect of the invention, wherein the second aqueous phase is 40 to 75 mass% of the total amount of the O/W emulsified composition. The method for producing an O/W emulsified composition according to any one of claims 1 to 3, wherein (A) the carbon number is 12 to 26 with respect to 10 parts by mass of the oil component. The total amount of the aliphatic alcohol and the (C) anionic surfactant is 0.5 to 10 parts by mass.