JP2912426B2 - Micronized emulsion composition - Google Patents

Description

The present invention relates to a liquid oily substance, a nonionic surfactant,
The present invention relates to a method for producing a finely divided emulsion composition by adding an ionic surfactant to an emulsion prepared by colliding a preliminary emulsion containing water.

More specifically, the present invention relates to a method for producing a finely divided emulsion composition having excellent skin safety, sensory characteristics, and storage stability, which can be used in the fields of cosmetics, pharmaceuticals, and the like.

[Problems to be solved by conventional technology and invention]

In general, a large amount of a surfactant is required to obtain a transparent composition by refining emulsified particles (oil: surfactant: 1: 5 to 20). ,
There are problems such as a decrease in sensory characteristics and skin safety.

As a method for solving this problem, Japanese Patent Publication No. 59-15005 discloses a method in which emulsified particles are made finer by causing emulsions to collide with each other or by causing the emulsion to collide with a vessel wall.

However, the resulting emulsion has excellent sensory properties and skin safety, but lacks stability, and cannot maintain a state in which particles are united or separated and finely divided by heating or aging. There is a disadvantage that.

Accordingly, an object of the present invention is to provide a method for producing a finely divided emulsion having good stability.

[Means for solving the problem]

The present invention relates to a method wherein: (a) an oily substance which is liquid at room temperature; (b) a nonionic surfactant having an HLB value in the range of 7.0 to 16.0; This is a method for producing a finely divided emulsion composition obtained by adding (d) a hydrophilic ionic surfactant to an emulsion having an average particle size of 10 to 200 nm obtained by colliding with a wall.

 Hereinafter, the configuration of the present invention will be described in detail.

The oily substance that is liquid at room temperature used in the present invention is an oil that exhibits a liquid state at normal temperature, such as liquid paraffin,
Squalane, liquid synthetic ester oils (isopropyl myristate, isopropyl palmitate, octyldodecyl myristate, etc.), vegetable oils (olive oil, soybean oil,
Rice bran oil, cottonseed oil, etc.), methylphenylpolysiloxane and the like. However, it is not limited to these. Liquid oily substances are used alone or in combination of two or more.

The content of these oily substances in the present invention is preferably 0.1 to 30% by weight based on 100% by weight (hereinafter abbreviated as wt%) of the total amount of the finely divided emulsion, but is not limited thereto.

Nonionic surfactant used in the present invention,
What is usually used as a raw material of cosmetics etc. may be used, and there is no particular limitation. For example, polyoxyethylene (hereinafter, referred to as POE) sorbitan monooleate, POE sorbitan monostearate, POE sorbitan fatty acid esters such as POE sorbitan trioleate, POE sorbit monooleate, POE sorbit pentaoleate, POE sorbit monostearate Fatty acid esters such as POE sorbitol fatty acid esters such as glycerin monostearate, POE glycerin monoisostearate, POE glycerin triisostearate, and glycerin fatty acids such as glyceryl monostearate and glyceryl monoisostearate POE fatty acid esters such as esters, POE monooleate, POE distearate, POE dioleate, POE oleyl ether, POE stearyl ether, POE behenyl ether, POE2-octyldodecyl ether, POE2
-POE alkyl ethers such as hexyldecyl ether, POE2-heptylundecyl ether, POE2-decyltetradecylether, POE2-decylpentadecylether, POE cholestanol ether, POE alkyl phenyl ethers such as POE nonylphenyl ether, POE・ POP block copolymers, POE ・ POP cetyl ether, POE ・ POP2-
POE / POP alkyl ethers such as decyltetradecyl ether, POE / POP hydrogenated lanolin, POE castor oil or hydrogenated castor oil derivatives such as POE castor oil, POE beeswax lanolin derivatives such as POE sorbit beeswax, sucrose oleic acid mono Examples include sugar esters such as esters, polyglycerin monoalkyl esters and monoalkyl ethers.

Among these nonionic surfactants, the HLB value is 7.0 to
Those having a HLB value in the range of 16.0 or adjusting the HLB value to 7.0 to 16.0 by combining two or more kinds are used.

The content of the nonionic surfactant in the present invention is about 0.1 to 30.0% by weight based on the total amount of the finely divided emulsion as 100, but the ratio with the oily substance is preferably in a range of 1: 0.5 to 5, and preferably in the range of 1: 0.5 to 5. The range of 1-3 is more preferable. If the ratio of the nonionic surfactant to the oily substance is small, a finely divided emulsion will not be formed, and if the content itself is large, skin safety and sensory characteristics will be poor. Examples of combinations of these nonionic surfactants and liquid oily substances passed through emulsification and dispersion include the following.

Of course, it is not limited to these combinations.

The water used in the present invention includes purified water such as distilled water, but is not limited thereto.

The water content in the present invention is about 40 to 99% by weight based on 100% by weight of the total amount of the finely divided emulsion.

In the present invention, as means for making the preliminary emulsion finer, there is, for example, injection by a nozzle. In this case, the injection pressure is, for example, 300 to 1000 kg / cm ² and the temperature is 5 to 40 ° C.
By setting in the range, the desired finely divided emulsion can be obtained. However, this differs depending on the machine, and is not particularly limited.

The average particle size of the finely divided emulsion in the present invention is 10
Although it is -200 nm, when it exceeds 200 nm, the appearance is inferior.

The hydrophilic ionic surfactant used in the present invention may be one usually used as a raw material for cosmetics and the like, and is not particularly limited. Examples of the anionic surfactant include fatty acid soaps such as sodium laurate and potassium palmitate; higher alkyl sulfates such as sodium lauryl sulfate and potassium lauryl sulfate; polyoxyethylene (hereinafter referred to as POE) lauryl sulfate triethanol; Alkyl ether sulfates such as amines, N-acyl sarcosine acids such as sodium lauroyl sarcosine, higher fatty acid amide sulfonates such as N-myristoyl-N-methyltaurine sodium, POE sodium oleyl ether phosphate, POE stearyl ether phosphate And the like, sulfosuccinates such as sodium di-2-ethylhexylsulfosuccinate, sodium linear dodecylbenzenesulfonate, triethanolamine linear dodecylbenzenesulfonate, lini Alkylbenzene sulfonates such as dodecylbenzene sulfonic acid, N- lauroyl glutamate monosodium, N- stearoyl glutamate disodium, N- acyl glutamates such as N- myristoyl -L- monosodium glutamate and the like.

Examples of the cationic surfactant include alkyl trimethyl ammonium salts such as stearyl trimethyl ammonium chloride and lauryl trimethyl ammonium chloride, dialkyl dimethyl ammonium salts, alkyl quaternary ammonium salts, and alkyl amine salts.

Examples of the amphoteric surfactant include 2-undecyl-
N, N, N- (hydroxyethylcarboxymethyl) -2-
Imidazoline amphoteric surfactants such as sodium imidazoline, 2-cocoyl-2-imidazolinium hydroxide-1-carboxyethyloxy disodium salt, 2-heptadecyl-N-carboxymethyl-N-hydroxyethylimidazolinium betaine, Betaine surfactants such as betaine lauryl dimethylaminoacetate, alkyl betaine, amido betaine and sulfobetaine, N-lauryl β
Amino acid salts such as -alanine, N-stearyl β-alanine,
And phospholipids such as lysolecithin.

These ionic surfactants are used alone or in combination of two or more.

The content of the hydrophilic ionic surfactant in the present invention is about 0.001 to 20.0 wt with respect to the total amount of the finely divided emulsion.
%, The ratio to the oily substance is preferably in the range of 1: 0.01 to 2.0, and more preferably 1: 0.1 to 1.0. If the content is small, the effect is small, and if the content is large, the effect is not improved correspondingly, and conversely, the skin safety and the sensory characteristics are reduced.

These hydrophilic ionic surfactants are added after the preparation of the micronized emulsion, and when added to the preliminary emulsion before the preparation of the micronized emulsion, the micronized emulsion desired in the present invention is not obtained. Even if a hydrophilic ionic surfactant is added to the finely divided emulsion, the average particle size does not change.

The finely divided emulsion of the present invention contains, in addition to the above essential components, dyes, fragrances, preservatives, pigments, antioxidants, thickeners, humectants, ultraviolet absorbers, chelating agents, other oils,
Surfactants, activation auxiliaries and the like can be appropriately compounded within a range that achieves the object of the present invention.

The micronized emulsion of the present invention is prepared, for example, as follows.

A nonionic surfactant is uniformly dissolved in an oily substance that is liquid at room temperature at room temperature or under heating. To this, water and other water-soluble components are added and mixed and stirred to obtain a preliminary emulsion. After finely pulverizing this with a microfluidizer or the like, a stable pulverized emulsion can be prepared by adding a hydrophilic ionic surfactant.

The method for producing a finely divided emulsion of the present invention can be applied to products such as lotions, hair tonics, hair oils, cleansing oils, aerosol products, and pharmaceutical solutions.

〔Example〕

Hereinafter, the present invention will be described in detail based on Examples and Comparative Examples.

The test methods for skin safety, sensory characteristics, and storage safety described in the examples are as follows.

(1) Skin safety test 0.05 g of a sample was applied to the skin on the flexion side of the forearm of 25 subjects.
After 24 hours of obstruction by using a patch test patch with a circular lint cloth of 1.0 cm, according to the following criteria,
For each sample, the skin condition of 25 subjects was evaluated and judged.

The judgment result was taken from the one with the strongest reaction after 1 hour and 24 hours after the bandage removal, and the evaluation was shown by the number of people (±) or more.

(2) Sensory property evaluation After 20 subjects continuously used the sample for 10 days, the property of the sample was evaluated.

The test results were expressed by the number of persons who answered, "No stickiness or sliminess", "Good compatibility with skin", and "Preferable oiliness".

(3) Storage stability test After storing the sample in a constant temperature room at 45 ° C for 2 weeks, observe the appearance of the sample. If no abnormality is observed (the appearance is transparent or translucent), mark ○. When x was observed (when oil separated or became cloudy, etc.), it was evaluated as x. Moreover, what was already cloudy at the time of preparation was set to xx.

(4) Measurement of average particle size Particle size distribution analyzer using photon correlation spectroscopy BI-90 (BROOKHAVEN INSTRUMENTS CORPOR)
ATION) was used to measure the average particle diameter immediately after preparation.

[Examples 1 to 14, Comparative Examples 1 to 4 Transparent lotion] Transparent lotion was prepared according to the composition shown in Table 1, and the above-described tests were performed.

(1) Composition (2) Preparation method The component (B) was uniformly dissolved in the component (A) at room temperature or by heating, and mixed. The component (C) was sequentially added thereto, followed by mixing and stirring to obtain a preliminary emulsion.

This was refined with a microfluidizer (Microfluidics) at 700 kg / cm ² at 30 ° C. (Comparative Examples 1 and 2).
After the addition of the finely divided emulsion, the component (D) was added.

With respect to Comparative Examples 3 and 4, the components (B) and (D) were uniformly dissolved in the component (A), mixed, and the component (C) was sequentially added thereto. After that, microfluidizer treatment was performed as described above.

(3) Properties As shown in Tables 4 and 5, Examples 1 to 14 obtained by the method for producing a finely divided emulsion of the present invention were applied to all of the skin safety test, the sensory property evaluation, and the storage stability test. hand,
Good evaluation was obtained.

In particular, it was clearly recognized that the storage stability of the micronized emulsion was significantly improved by adding a small amount of a hydrophilic ionic surfactant after the microfluidizer treatment.

In contrast, Comparative Example 1, which was not subjected to the microfluidizer treatment, had a large average particle size and was already clouded at the time of preparation. Further, Comparative Example 2 containing no hydrophilic ionic surfactant had a small particle size immediately after preparation, but became cloudy when stored for 2 weeks. Comparative Examples 3 and 4 in which a hydrophilic ionic surfactant was added before microfluidizer treatment
Was already clouded at the time of preparation because it was not refined and had a large average particle size.

[Effects of the Invention] As described above, the present invention has a much smaller amount of nonionic surfactant than conventional solubilizing systems, and can incorporate a large amount of oily components, has high skin safety, and has organoleptic properties. It is apparent that the present invention provides a method for producing a finely divided emulsion composition which is excellent in storage stability and storage stability.

Claims (1)

(57) [Claims] 1. Preliminary emulsions comprising (a) an oily substance which is liquid at room temperature, (b) a nonionic surfactant having an HLB value in the range of 7.0 to 16.0, and (c) water collide with each other or A method for producing a finely divided emulsion composition obtained by adding (d) a hydrophilic ionic surfactant to an emulsion having an average particle size of 10 to 200 nm obtained by colliding the emulsion with a wall.