JPS5935362B2 - Composition of skin emulsion - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a non-viscous acidic skin emulsion composition that provides moderately good astringency, moisturizing, smoothness, and bactericidal effect to the skin and has excellent storage stability.

Conventionally, skin emulsions containing higher alkyl sulfate ester salts irritate the skin, and even if they contain cholesterol, etc., they tend to cause hydrolysis on the acidic side (PH 4 to 6.0), resulting in a decrease in emulsion stability. There were drawbacks.

The present inventor has conducted intensive research to improve the drawbacks of skin emulsions containing higher alcohol sulfate ester salts or cholesterol. The skin emulsion that is a mixture of the higher alcohol sulfate ester salt of formula (2), cholesterol, and water prevents the hydrolysis reaction of the higher alcohol sulfate ester salt even on the acidic side, and the emulsion stability during long-term storage is significantly improved. The present invention has been completed based on the discovery that it has been improved and can also provide a moisturizing feeling, smoothness, astringent property, and bactericidal effect without irritating the skin during use.

The purpose of the present invention is to provide a skin emulsion composition that has excellent emulsion stability and storage stability, and provides a moderately good moist feeling, smoothness, astringency, and bactericidal effect without irritating the skin during use. It's about doing.

The present invention relates to the following - Crotch 1) (In the above formula, R is an alkyl group or alkenyl group having 6 to 17 carbon atoms, R' is a benzyl group, 4-nitrobenzyl group, 3,4-dichlorobenzyl group) , 4-chlorobenzyl group, 2,4-dichlorobenzyl group, methylbenzyl group, or methyl group) in an amount of 0.025 to 0.05% by weight (% by weight is based on the weight of the composition). standard.

Same hereinafter), cholesterol is 0.1 to 2.0% by weight,
The following general formula (2) % formula % (2) (In the above formula, R is an alkyl group or alkenyl group having 11 to 18 carbon atoms, A is sodium, potassium or NH
The higher alcohol sulfate ester salt represented by , is 0.1~
2% by weight, 1 to 20% by weight of liquid hydrocarbons, and 0.2% of common salt.
This is a skin emulsion composition characterized by containing 0.05 to 0.5% by weight and 75 to 98% by weight of water.

The specific quaternary ammonium salts used in the present invention are those represented by 1) above, and may be used singly or in combination of two or more.

The blending amount (hereinafter referred to as content) is 0.025 to 0.05% by weight, preferably 0.025% to 0.05% by weight, based on the total weight of the prescription components (hereinafter referred to as relative to the weight of the composition).
03 to 0.04% by weight.

If it is less than 0.025% by weight, the emulsion stability and storage stability of the composition will tend to decrease, and if it is more than 0.05% by weight, it will tend to have strong pungent properties.

Among the quaternary ammonium salts represented by the general formula (1), particularly preferred are lauryldimethylbenzylammonium chloride, octyldimethylbenzylammonium chloride, lauryldimethyl 4-nitrobenzylammonium chloride, lauryldimethyl 3,4- These include dichlorobenzylammonium chloride, lauryldimethyliso-dichlorobenzylchloride, lauryltrimethylammonium chloride, and the like.

The content of cholesterol is 0.1 based on the weight of the composition.
-2% by weight, preferably 0.3-1.5% by weight.

If the amount is less than 0.1% by weight, emulsion stability and storage stability will decrease, and if it is more than 2% by weight, it will be difficult to produce a stable non-viscous emulsion.

The higher alcohol sulfate ester salts used in the present invention are those represented by the general formula (2), and include randesicyl alcohol sulfate, lauryl alcohol, sulfate, tritacyl alcohol sulfate, myristyl alcohol sulfate, and pentadecyl alcohol sulfate. Preferable examples include sodium salt, potassium salt, or ammonium salt of ester, cetyl alcohol sulfate, heptadecyl alcohol sulfate, oleyl alcohol sulfate, and stearyl alcohol sulfate.

Higher alcohol sulfate ester salts can be used singly or in combination of two or more, and the amount used (content) is as follows:
0.1 to 2% by weight, preferably 0.1% to 2% by weight, based on the weight of the composition.
It is 3 to 1.5% by weight.

If the amount is less than 0.1% by weight, emulsion stability and storage stability will decrease, and if it is more than 2% by weight, it will be difficult to form a non-viscous emulsion.

The content of salt is 0.05 to 0.5 based on the weight of the composition.
% by weight, preferably 0.1-0.3% by weight.

When the amount is less than 0.05% by weight, storage stability decreases,
If the amount is more than 0.5% by weight, the user will feel a strong sense of discomfort and the storage stability will tend to decrease.

Liquid hydrocarbons include liquid paraffin, squalane,
Psostane, hydrogenated polyisoprene, carbon number 3~
Oligomers of No. 12 olefins or hydrogenated products thereof are preferred.

The content of liquid hydrocarbon is 1 to 20% by weight of the composition.
Weight%.

Preferably it is 3 to 15% by weight.

If it is less than 1% by weight, it will not function as a skin emulsion (emulsion stability and storage stability will tend to decrease,
If it exceeds 20% by weight, viscosity will appear and it will be difficult to obtain an acidic, non-viscous material.

The water content is between 75 and 98% by weight, based on the weight of the composition.

Preferably it is 81.5 to 96.0% by weight.

When it is less than 75% by weight, stability tends to decrease under low temperatures such as in winter, and when it exceeds 95% by weight, stability tends to decrease under high temperatures such as during summer.

The composition of the present invention is prepared by heating a solution consisting of a required amount of liquid hydrocarbon, cholesterol into a heated homogeneous solution, salt, water, a quaternary ammonium salt, and a higher alkyl sulfate salt, and then heating the solution with stirring. It is manufactured by mixing, emulsifying and dispersing.

The skin emulsion composition of the present invention is an acidic, non-viscous liquid, and the coexisting salt also acts as a stabilizer, resulting in an emulsion that has excellent long-term storage stability and does not separate even after 2 years of storage. do not become.

However, as will be described later, in a case other than the present invention in which <CI- is replaced with Br-, the hydrolysis of the higher alkyl sulfate ester salt cannot be inhibited.

In this way, as will be described later, the effect of the coexistence of common salt and the quaternary ammonium salt having the specific structure is extremely unique.

The present invention will be explained in detail below.

Note that "part" means part by weight, and "%" means percent by weight.

Example 1 (1) Composition of the skin emulsion of the present invention 1, liquid paraffin (pure) 5 parts 2, cholesterol (pure) 0.5 parts 3, lauryldimethylbenzylammonium chloride (pure) 0.05 parts 4 , common salt (purified salt) 0.1 part 5, cetyl sulfate sodium ester (purity) 0.7 part 6, fragrance pigment appropriate amount 7, water
93. 3 parts total ioo parts (2) Production of skin emulsion composition Dissolve cholesterol in liquid paraffin by heating (A
) was prepared.

Next, common salt and lauryldimethylbenzyl ammonium chloride are added to water, heated, and added with cetyl sulfate sodium ester to create a homogeneous mixed solution, which has excellent long-term storage stability and does not become an emulsion that will separate even after 2 years of storage.

However, as in Comparative Example described later, a product (B) other than the present invention was prepared in which the chlorine atom of the quaternary ammonium salt of the above general formula was replaced with a bromine atom even when doucleate salt was present.

(B) was added to the mixed solution with stirring, and after mixing, perfume and pigment were added and cooled to room temperature while stirring to obtain a skin emulsion composition of the present invention.

(3) Comparative Example Skin Emulsion Composition ■ Comparative Example 1 was carried out in the same manner as in the present invention except that lauryl dimethyl benzyl bromide was used instead of lauryl dimethyl benzyl chloride.

(2) Comparative Example 2 was carried out in the same manner as in the present invention except that phytosterol was used instead of cholesterol.

(2) Comparative Example 3 was carried out in the same manner as in the present invention except that triethanolammonium stearate was used in place of sodium cetyl sulfate.

(2) Comparative Example 4 was carried out in the same manner as in the present invention except that lauryldimethylbenzylammonium chloride was not used.

(2) Comparative Example 5 was carried out in the same manner as in the present invention except that only common salt was not used.

(4) Next, the storage stability, appearance, fading test, and sensory test (skin compatibility, skin smoothness, moist feeling, and irritation) of the compositions of the present invention examples and comparative examples were examined.

The results are shown in Table 1. In addition, the appearance in Table 1 is observed by naked eye, and the storage stability is stable if the emulsion is uniform when stored in a constant temperature room for 6 months at -10℃ with a 2-week cycle; The case was considered unstable.

A sensory test was conducted with a panel of 20 women, and the numbers are the number of people who answered that everything was good except for the stimulation.

The fading test was conducted by visual judgment of the color after 4 hours of fading using a fetometer test.

As is clear from the results, the composition of Example 1 of the present invention is significantly superior in uniform emulsifying properties, storage stability, and functionality compared to the composition of Comparative Example.

Even if similar components are used in place of the constituent components of the present invention, a good non-viscous acidic emulsion composition cannot be obtained.

Example 2 The same procedure as in Example 10 of the present invention was conducted except that the content of lalaryl dimethylbenzylammonium chloride was changed as shown in Table 2.

The results are shown in Table 2.

As is clear from this result, the content of the specific quaternary ammonium salt is 0.025 to 0.05%.

Animal Skin Irritation Test According to the method of Draize, a patch piece coated with 0.5 ml of the test sample is applied to the skin of white domestic rabbits (three rabbits were used) whose back hair has been shaved.

Cover with rabbit rubber clothing and secure in the animal cage to prevent movement.

After 24 hours, the patch pieces are removed and the degree of reaction is recorded according to the criteria below.

Further, the determination is also made after 72 hours, and the average score after 24 hours and after 72 hours is calculated and used as the irritation score.

Judgment (1) No erythema or skin formation erythema 0 Very slight erythema 1 Visible erythema 2 Moderate to severe erythema 3 Severe erythema and slight skin formation 4 (2) Formation of edema No edema 0 Very slight edema 1 Slight edema 2 Moderate edema 3 Severe edema 4 Based on the calculated score, the degree of irritation is evaluated as follows.

0-2 Slight irritation or almost no irritation Hoof 12
5 or more Moderate irritation 5 or more Strong irritation Example 3 The same procedure as in Example 10 of the present invention was conducted except that the cholesterol content was changed as shown in Table 3.

The results are shown in Table 3.

As is clear from the results above, when the cholesterol content is less than 0.1% or more than 2%, the stability deteriorates, and within the range of 0.3 to 1.5%, a non-viscous acidic emulsion is produced. can be obtained.

*Example 4 The same procedure as Example 1 of the present invention was conducted except that the salt content was changed as shown in Table 4.

The results are shown in Table 4.

As is clear from this result, the salt content is 0.05%.
If the amount is less (or more than 0.5%), uniform emulsification cannot be obtained.

Example 5 Instead of lauryldimethylbenzylammonium chloride, as quaternary ammonium salts, stearyltrimethylammonium chloride (A1), cetyltrimethylammonium chloride (A2), n-octyltrimethylammonium chloride (A3), and capryltrimethylammonium chloride (A4) were used as quaternary ammonium salts. ), capryldimethylbenzylammonium chloride (A5), oleyldimethylbenzylammonium chloride (A6), 2
-Ethylhexyldimethylbenzylammonium chloride (A7'), octyldimethylbenzylammonium chloride (A8), cetyldimethylbenzylammonium chloride (A9), lauryl dimethyl 4-
nitrobenzyl ammonium chloride (A, 10),
Lauryldimethyl 2,4-dichlorobenzylammonium 20lide (All), lauryldimethylmethylbenzylammonium chloride (A12), lauryldimethyl 3,4-dichlorobenzylammonium chloride (A13), lauryldimethyl 4-chlorobenzylammonium chloride (A14) The same procedure as in Example 1 of the present invention was carried out except that .

The results are shown in Table 5. Example 6 (When using a liquid hydrocarbon other than liquid paraffin) Instead of liquid paraffin, squalane, a hydrogenated polyisobutylene, a hydrogenated polyisoprene, a synthetic stanrane (Pamit 40 from Lion Oil KK product), Polymer of octene-1 (viscosity 305CPS1 acid value 0.01
, pour point ~40℃, this is α-olefin polymerized oil),
Dodecene-1 polymer (viscosity 190CPS, acid value 0.0
1. Pour point -40℃, this is α-offine polymerized oil) pristane, 2, 6, 15, 19, 23-hexamethyltetracosane, liquid polyisobutylene (viscosity at 100'P is 20C8T, average molecular weight 320 , odorless) Liquid polyisobutyne (viscosity at 100'F is 18C8T, average molecular weight 392, odorless), LIPO-LUBE2O8 (Lion oil product: α-olefin polymerized oil, kinematic viscosity is 17
．． The same procedure as in Example 10 of the present invention was conducted except that 87/37.8°C Stokes, specific gravity 0.818, and viscosity index 124) were used.

As a result, all skin emulsion compositions had a uniform emulsion appearance, stable storage stability after 6 months with no abnormalities, no change in fading test, 16 people found that the skin blended well with the skin, and 17 people found the skin smooth. , 17 people felt moist, and the irritation was O, PH.
It was 4.5 to 4.7.

Claims (1)

[Scope of Claims] 1 The following - Crotch meat 1) (In the above formula, R is an alkyl group or alkenyl group having 6 to 17 carbon atoms, R' is a benzyl group, 4-nitrobenzyl group, 3,4- Dichlorobenzyl group, 4-chlorobenzyl group. 2.4-) Chlorohensyl group, methylbenzyl group or methyl group. ) Quaternary ammonium salt represented by 0.025 to 0
．． 05% by weight (weight% is based on the weight of the composition. The same applies hereinafter), cholesterol 0.1 to 2.0% by weight,
Below - Crotch meat 2) RO8O3A ・・・・・・・・・・・・・・・・・・
...... (2) (In the above formula, R has 11 to 11 carbon atoms
18 alkyl or alkenyl group, A is sodium, potassium, or NH4) The higher alcohol sulfate salt represented by te is 0.1 to
2% by weight, 1 to 20% by weight of liquid hydrocarbons, and 0.2% of common salt.
A skin emulsion composition characterized in that it contains 05 to 0.5% by weight and 75 to 98% by weight of water.