KR20190089496A - Preparation method of cleansing cosmetic composition using eutectic point and the compostion - Google Patents

Abstract

The present invention provides a method for producing a cleansing cosmetic composition comprising fatty acids and polyols, and the composition. More specifically, the present invention provides a method for producing a composition having a stable crystal structure using the eutectic point of fatty acids. According to the present invention, after mixing, as fatty acids, myristic acids and stearic acids in a weight ratio of 2.5 to 8 : 1, and then mixing the polyols, it is possible to produce a foam cleanser having stabilized physical properties even at high temperatures.

Description

The present invention relates to a method of preparing a cleansing cosmetic composition using a eutectic point and a method of preparing the cleansing cosmetic composition using the eutectic point and the compostion,

The present invention relates to a method for producing a cleansing cosmetic composition using a eutectic point and to the composition.

The makeup cleansing product consists of a primary cleanser such as cleansing oil and water, and a secondary cleanser containing a cream type cleansing foam. In order to makeup cleansing, a double cleanser is known as a basic. However, A cleansing foam has been used basically.

Cream-type fatty acid soaps, commonly known as cleansing foams, were first developed in the 1960s and began to appear on the market. They are a facial-only product with a high level of moisturizing and skin protection in addition to the excellent cleaning and foaming power of soap . Since the formulation of the cleansing foam is in a creamy state, it has a merit that it can obtain a rich foam compared to a hard soap bar, and has developed a lot as an important cleanser for cosmetics. Currently, And the like.

The formulation of the cleansing foams is a mixture of 12 to 18 carbon fatty acids (stearic acid, palmitic acid, myristic acid, lauric acid, etc.), known to be highly cleansing, a mixture of potassium hydroxide, polyol (glycerin, (Such as glycerin, glycerin, glycerin, glycerin, glycerin, glycerin, glycerin, glycerin, Elasticity, persistence, cleaning power, etc.), physical properties and stability. However, it is difficult to obtain a stable cream soap with only a fatty acid and potassium hydroxide, and the use of a polyol and a nonionic or anionic surfactant is essential for controlling physical properties and improving stability.

The cleansing foam is made of crystal gel structure and is weak against shear stress unlike emulsifying system and easily separates at high temperature storage condition. Thus, conventional cleansing foams have a problem of deteriorating the quality of formulations, such as crystallization, which is easily broken by shear stress and is separated at high temperature, because the neutralized fatty acid determines the foaming power and forms hardness with the free fatty acid Respectively.

In order to solve the above-mentioned problems, the inventors of the present invention have found that, in a method of manufacturing a cleansing cosmetic composition containing a fatty acid and a polyol, the fatty acid is mixed at a ratio showing the most stable structure at the eutectic point of the fatty acid, , It was confirmed that the production of fatty acid crystals was inhibited at a high temperature condition when the cleansing cosmetic composition was prepared, thereby completing the present invention.

Korean Patent No. 10-1404969

The present invention provides a method for producing a cleansing cosmetic composition comprising a fatty acid and a polyol, and a method for producing a cleansing cosmetic composition having a stable crystal structure using the eutectic point of a fatty acid.

In order to solve the above problems, the inventors of the present invention have conducted intensive studies to produce a cleansing cosmetic composition having a composition having a stable formulation, and as a result, discovered that a cosmetic composition having a rigid structure can be obtained by mixing a fatty acid and a polyol, Completed

Thus, in one embodiment, the invention provides a method of making a cleansing cosmetic composition comprising the steps of:

(S1) mixing the myristic acid and the stearic acid and heating them to prepare a fat portion;

Mixing the neutralizing agent, the polyol and the purified water and stirring to prepare a water phase (S2); And

(S3) of injecting the water phase of step S2 into the upper part of the fat of step S1 and then stirring to prepare a cleansing cosmetic composition.

In the production method of the present invention, the myristic acid and the stearic acid may be mixed at a weight ratio of 2.5 to 8: 1.

In the production method of the present invention, the neutralizing agent is added so that the neutralization ratio to the acid value of the fatty acid portion is 70 to 80%.

In addition, the neutralizing agent is characterized by being at least one neutralizing agent selected from the group consisting of potassium hydroxide, sodium hydroxide, magnesium hydroxide, triethanolamine, tromethamine, arginine, and amino methylpropanol.

The production method of the present invention is characterized in that the polyol is contained in an amount of 20 to 50% by weight based on 100% by weight of the total composition.

The polyol may be at least one selected from the group consisting of glycerin, polyethylene glycol, dipropylene glycol, propylene glycol, butylene glycol, raffinose, inositol, sorbitol, and maltitol.

The production method of the present invention may further include but is not limited to further comprising an anionic surfactant, a cationic surfactant or an amphoteric surfactant.

Further, as another embodiment of the present invention, there is provided a lipid upper part comprising myristic acid and stearic acid; And a water-soluble part including a neutralizing agent, a polyol, and purified water.

In the process for preparing a cosmetic composition according to the present invention, the ratio of myristic acid to stearic acid is maintained at 3: 1, and glycerin is added in a high content to increase the crystal firmness, shear stress, a cleansing cosmetic composition having a relatively stable formulation can be prepared.

1 shows the DSC graphs of eutectic points of Experimental Examples 1 to 5 prepared according to the present invention. (A) (B) is a graph showing the results of DSC measurement of the crystals obtained after preserving Production Examples 1-1 to 1-6 at 37 占 폚 for 2 weeks. Fig.
2 is a diagram showing the results of high-temperature stability optical images of Comparative Examples and Examples prepared according to the present invention.
FIG. 3 is a microscopic optical image of crystals obtained in Comparative Examples and Examples prepared according to the present invention.

The present invention will now be described more fully hereinafter with reference to the accompanying drawings, in which the present invention may be practiced. It will be apparent, however, to one skilled in the art that the present invention may be embodied in many different forms and is not limited to the embodiments described herein.

That is, the present invention relates to a method for producing a cosmetic composition containing a fatty acid, wherein a composition ratio of myristic acid and stearic acid is 2.5 to 8: 1 and glycerin is added to the polyol, Of the present invention.

In addition, the phase behavior of the crystal gel structure was investigated by DSC (differential scanning calorimeter) measurement in water / neutralizer / fatty acid system according to fatty acid mixture ratio, neutralization degree and various polyols. DSC is used as a very useful tool for studying phase behavior of emulsified products, and it is considered to be a suitable device for understanding the crystal structure that varies depending on various factors, and was utilized in the present invention analysis.

Existing cleansing foams have a weak crystal structure with shear stress, which indicates severe physical properties such as low hardness during filling and high hardness at high temperature. Accordingly, the present inventors have studied various polyols in a cosmetic composition containing a fatty acid, and have found that glycerin affects the crystal formation, thereby producing a cosmetic composition stable to formulation stability and shear stress.

Specifically, when the ratio of myristic acid to stearic acid in the fatty acid is in the range of 3: 1, each of the crystals has a eutectic point in which the crystals are present in the same crystal as one compound. When a large amount of glycerin is contained, And a cosmetic composition containing a fatty acid having a crystal structure stable to shear stress can be prepared, thereby completing the present invention.

Accordingly, the present invention provides a process for preparing a cleansing cosmetic composition comprising the steps of:

(S1) mixing the myristic acid and the stearic acid and heating them to prepare a fat portion;

Mixing the neutralizing agent, the polyol and the purified water and stirring to prepare a water phase (S2); And

(S3) of injecting the water phase of step S2 into the upper part of the fat of step S1 and then stirring to prepare a cleansing cosmetic composition.

The present invention also relates to a topical composition comprising myristic acid and a stearic acid; And a water phase portion comprising a neutralizing agent, a polyol, and purified water.

The myristic acid and the stearic acid can be mixed in a weight ratio of 2.5 to 8: 1, and when having a weight ratio of 2.5 to 5.5: 1, the smallest entropy difference is observed, The results are shown in Example 1. More preferably at a weight ratio of 3: 1.

It is preferable that the neutralizing agent is added in such a manner that the neutralization ratio with respect to the acid value of the fatty acid portion is 70 to 80%, and when the neutralization ratio is less than 70%, a large amount of non-neutralized crystalline fatty acid is contained, It is difficult to obtain a foamability that can be expected from a detergent, and when it exceeds 80%, it can be realized as a liquid phase because there are few fatty acid crystals for maintaining the appearance and hardness of the cream phase It may be inappropriate.

The neutralizing agent is one, such as the any neutralizing agent commonly used in the art and can include, specifically, potassium hydroxide (KOH), sodium hydroxide (NaOH), magnesium hydroxide (Mg (OH) ₂₎ A neutralizing agent such as triethanolamine, tromethamine, arginine, aminomethylpropanol and the like may be used. A single or a mixture of the neutralizing agents may be used, but the present invention is not limited thereto no.

Further, the myristic acid and stearic acid of the present invention are fatty acids. In the production method and composition of the present invention, the kind of the fatty acid may include any fatty acid conventionally used in the art besides myristic acid and stearic acid. Specifically, it may be a fatty acid corresponding to the following formula (1). However, it is preferable to use Myristic acid and Stearic acid according to the mixing ratio provided in the present invention as in the embodiment of the present invention from the viewpoint of crystal stability.

[Chemical Formula 1]

C _n H _{2n + 2} O ₂

Wherein C is a linear or branched C ₈ -C ₂₂ alkyl radical or a mixture of radicals, n is an integer or binary number (average value) which can be from 8 to 26, preferably from 12 to 18, and is saturated or unsaturated Fatty acids may be included, and a single or a mixture of compounds of formula (1) may be used. For example, saturated fatty acids, omega-3 fatty acids, omega-6 fatty acids, omega-7 fatty acids, and omega-9 fatty acids, and the above-mentioned materials are merely examples and are not limited to the above and can be used singly or in combination .

The polyol is contained in an amount of 20 to 50% by weight based on 100% by weight of the total composition, and includes a large amount of the polyol in the composition of the present invention as compared with the conventional cleansing foam composition. When the polyol is contained in an amount less than 20% by weight, the fluidity may fall and the stability may be lowered. When the polyol is contained in an amount exceeding 50% by weight, the enthalpy increases due to an increase in fluidity, .

The polyol may be at least one selected from the group consisting of glycerin, polyethylene glycol (glycereth-26, pegi-32, methylglucose-20, pegi-8, pegi-75, methylglucose- Lactol, butylene glycol, inositol, sorbitol, maltitol or raffinose, and it is advantageous to use a glycerin as in the embodiment of the present invention to have a stable crystal structure.

The composition may further comprise an anionic surfactant, a cationic surfactant or an amphoteric surfactant. As the kind of the surfactant, any surfactant conventionally used in the art can be used.

The cleansing cosmetic composition of the present invention is prepared in the form of a cream, and it is preferable that the cleansing cosmetic composition is produced in the form of a cream considering the usability of the cleansing foam, but the present invention is not limited thereto. For example, it may additionally be formulated into solutions, suspensions, emulsions, gels, soaps, oils, sprays and the like, but is not limited thereto. More specifically, it may be manufactured in the form of a product such as a cleansing cream, a cleansing foam, a cleansing water, a cleansing pack, or a cleansing spray, but is not limited thereto.

In the present invention, the fatty acid has a stable crystal at -20 ° C to 55 ° C. As in the present invention, the fatty acid in which the myristic acid and the stearic acid are 3: 1 has a melting point melting point, so crystals melt and exist as a liquid phase when the temperature exceeds 55 ° C. In addition, if the temperature is lower than -20 占 폚, crystals of solid form can be formed, and a cream form can not be formed.

According to the experimental example of the present invention, it was confirmed that the stability of the formulation stability was confirmed through the confirmation of the eutectic point of the fatty acid. As a result, it was confirmed that a relatively stable crystal was formed when the ratio of myristic acid and stearic acid was 3 to 5: 1 1 and Fig. 1).

Therefore, since a stable foam structure can not be formed simply at a temperature of 45 占 폚 or higher as a eutectic point, a method of stabilizing an additional crystal structure using a polyol has been devised.

As a result of Experimental Example 2 of the present invention, when glycerin is contained as an effective ingredient as a raw material for crystal growth in a cosmetic composition containing a fatty acid, a stable crystal structure is formed under a high temperature condition. (See Figs. 2 and 3).

Hereinafter, the present invention will be described in detail with reference to Examples. It is to be understood by those skilled in the art that these examples are for illustrative purposes only and that the scope of the present invention is not construed as being limited by these examples.

[Example]

Hereinafter, the present invention will be described in more detail with reference to Examples. These embodiments are only for illustrating the present invention, and thus the scope of the present invention is not construed as being limited by these embodiments.

Manufacturing example  1: Preparation for confirmation of the eutectic point of a cleansing composition containing a fatty acid

Production Examples 1-1 to 1-6 were prepared through the compositions shown in Table 1 below to confirm eutectic points. Specifically, myristic acid and stearic acid were heated and dissolved at a temperature of 70 to 80 ° C to prepare an A phase (upper lipid), and purified water and potassium hydroxide were heated to 70 to 80 ° C and stirred B phase (aqueous phase) was prepared.

The B phase was added to the A phase and stirred, followed by cooling and stirring to room temperature. The cleansing composition containing the fatty acid was prepared by adjusting the neutralization ratio of potassium hydroxide to potassium hydroxide to 73% to 76% in comparison with the acid value of A according to the general cleansing form neutralization ratio. As a result, an opaque creamy cleansing foam was produced.

Production Example 1-1 Production Example 1-2 Production Example 1-3 Production Example 1-4 Production Example 1-5 Production Example 1-6 A Myristic acid 22.0 20.0 18.0 20.0 21.0 22.0 A Stearic acid 2.0 4.0 6.0 10.0 15.0 22.0 B Purified water To 100 To 100 To 100 To 100 To 100 To 100 B Potassium hydroxide 4.8 4.7 4.5 5.7 6.7 8.0

Experimental Example  1: Confirmation of eutectic point of cleansing composition containing fatty acid

The cleansing foams of Production Examples 1-1 to 1-6 prepared in Preparation Example 1 were measured for their melting points using DSC. It has been confirmed that DSC measurement is not easy because it exists in the form of a liquid phase because it is above the melting point of the free fatty acid at a temperature of 45 캜 or higher.

The enthalpy values of the cleansing foams stored at room temperature for one week and the enthalpy values of the cleansing foams stored at 37 ℃ for 2 weeks were compared. As a result, as shown in Fig. 1 and Table 2, it was confirmed that the difference in enthalpy comparison was the smallest in Production Example 1-3 in which the ratio of myristic acid to stearic acid was 3: 1.

A B | B-A | Production Example 1-1 22.25 11.62 10.63 Production Example 1-2 22.02 20.32 1.7 Production Example 1-3 21.90 22.19 0.29 Production Example 1-4 24.13 13.35 10.78 Production Example 1-5 21.49 8.058 13.432 Production Example 1-6 21.27 7.475 13.795

Enthalpy is a unit of thermodynamic energy, useful information that can be used to describe the relative strength of chemical bonds, the nature of different atoms, and whether a specific reaction can occur. In particular, the degree of anxiety of the compound can be confirmed by the amount of enthalpy change when the change occurs.

From the above results, it is confirmed that the above result is due to the existence of a stable crystal structure by forming a eutectic point which forms one kind of compound when the free fatty acids of myristic acid and stearic acid exist in a certain ratio.

Manufacturing example  2: Preparation of Cleansing Composition Containing Fatty Acids

Thus, a cleansing composition was prepared according to the composition shown in Table 3 below, in order to confirm the stability of the composition of Example 1-3 except that polyol glycerin was not added (Comparative Example) and glycerin was added (Example).

Similar to Production Example 1, the A phase (upper lipid) was dissolved by heating at 70 to 80 ° C, and the B phase (aqueous phase) was mixed and stirred constantly at 70 to 80 ° C. After stirring, the mixture was cooled to room temperature and stirred. The cleansing composition was prepared by adjusting the neutralization ratio of potassium hydroxide to potassium hydroxide to 73 to 76% in comparison with the acid value of A according to the general cleansing form neutralization ratio.

Comparative Example Example A Myristic acid 27.0 27.0 A Stearic acid 9.0 9.0 B Purified water To 100 To 100 B Potassium hydroxide 7.0 7.0 B glycerin - 20.0

Experimental Example  2: Evaluation of formulation stability of cleansing composition containing fatty acid

In order to confirm the stability of a cleansing cosmetic containing a fatty acid and a polyol, the stability of Comparative Examples and Examples was evaluated in Experimental Example 2. Specifically, the stability of the comparative example and the example 1 of the present invention was confirmed by a method of storing the sample in a refrigerator for 4 weeks at room temperature, 45 ° C, and 50 ° C for 4 weeks, and the results are shown in Table 4 and FIG.

Experiment Item Comparative Example Example cold storage 1 week ○ ○ cold storage 2 weeks ○ ○ cold storage 4 weeks ○ ○ Room temperature 1 week ○ ○ Room temperature 2 weeks ○ ○ Room temperature 4 weeks ○ ○ 37 ℃ 1 week ○ ○ 37 ℃ 2 weeks ○ ○ 37 ℃ 4 weeks ○ ○ 45 ° C 1 week △ △ 45 ° C 2 weeks ○ ○ 45 ° C 4 weeks ○ ○ 50 ℃ 1 week △ △ 50 ℃ 2 weeks ○ ○ 50 ℃ 4 weeks ○ ○

?: Good,?: Difference from the beginning, X: Property change (separation, suspension, crystal precipitation, hardness change)

As a result, as shown in Table 4, in Comparative Examples and Examples, melting of crystals at 45 ° C and 50 ° C was observed at 1 week, but both cases showed the same appearance until 4th week. However, when the samples were allowed to stand at room temperature, there was a difference in crystal formation time.

FIG. 2 shows a state in which a sample at a high temperature has been left at room temperature for 5 minutes. Since the comparative example has a crystal structure, crystals precipitate rapidly due to the lowering of the solubility of the free fatty acid upon standing at room temperature, It can be seen that crystallization is performed slowly with similar physical properties as immediately after leaving at room temperature at a high temperature even after the lapse of the same time as the comparative example. This means that the external temperature change is more stable than the crystal structure of the existing cleansing foam.

Experimental Example  3: Determination of crystal structure of cleansing composition containing fatty acids

After preparing Comparative Examples and Examples, the compositions at room temperature were observed by a polarizing microscope and Cryo-SEM (cryogenic scanning electron microscopy).

As a result, as shown in FIG. 3, the comparative example has a needle-like structure with a smaller number of crystals than the examples. However, it can be seen that the crystals of the comparative example are grown more than the comparative example. This suggests that glycerin helps the formation of a multilamellar structure, which makes the crystal structure relatively stable to shear stress.

Therefore, the cleansing foam prepared by the production method of the present invention has a stable crystal structure, and when the cleansing foam is manufactured by the production method of the present invention, the cleansing foam is excellent in high-temperature and shear stress It was confirmed that a cleansing foam can be produced.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments. It belongs to the scope of right.

Claims (14)

A method for preparing a cleansing cosmetic composition comprising the steps of:
(S1) mixing the myristic acid and the stearic acid and heating them to prepare a fat portion;
Mixing the neutralizing agent, the polyol and the purified water and stirring to prepare a water phase (S2); And
(S3) of injecting the water phase of step S2 into the upper part of the fat of step S1 and then stirring to prepare a cleansing cosmetic composition.
The method according to claim 1,
Wherein the myristic acid and the stearic acid are mixed at a weight ratio of 2.5 to 8: 1.
The method according to claim 1,
Wherein the neutralizing agent is added so that the neutralization ratio to the acid value of the fatty acid portion becomes 70 to 80%.
The method according to claim 1 or 3,
Wherein the neutralizing agent is at least one neutralizing agent selected from the group consisting of potassium hydroxide, sodium hydroxide, magnesium hydroxide, triethanolamine, tromethamine, arginine, and amino methylpropanol. ≪ / RTI >
The method according to claim 1,
Wherein the polyol is contained in an amount of 20 to 50% by weight based on 100% by weight of the total composition.
6. The method according to claim 1 or 5,
Wherein the polyol is at least one selected from the group consisting of glycerin, polyethylene glycol, dipropylene glycol, propylene glycol, butylene glycol, raffinose, inositol, sorbitol and maltitol. ≪ / RTI >
The method according to claim 1,
Wherein the composition further comprises an anionic surfactant, a cationic surfactant or an amphoteric surfactant.
Fat tops comprising myristic acid and stearic acid; And
And a water phase containing a neutralizing agent, a polyol and purified water.
Cleansing cosmetic composition.
9. The method of claim 8,
Wherein the myristic acid and the stearic acid are mixed at a weight ratio of 2.5 to 8: 1.
9. The method of claim 8,
Wherein the neutralizing agent is contained so that the neutralization ratio to the acid value of the fatty acid portion is 70 to 80%.
11. The method according to claim 8 or 10,
Wherein the neutralizing agent is at least one neutralizing agent selected from the group consisting of potassium hydroxide, sodium hydroxide, magnesium hydroxide, triethanolamine, tromethamine, arginine, and amino methylpropanol. Composition.
9. The method of claim 8,
Wherein the polyol is contained in an amount of 20 to 50% by weight based on 100% by weight of the total composition.
The method according to claim 8 or 12,
Wherein the polyol is at least one selected from the group consisting of glycerin, polyethylene glycol, propylene glycol, dipropylene glycol, butylene glycol, raffinose, inositol, sorbitol and maltitol. .
9. The method of claim 8,
Wherein the composition further comprises an anionic surfactant, a cationic surfactant or an amphoteric surfactant.

Images