KR20190088026A - Nano emulsion composition comprising nano-cellulose and producing method thereof - Google Patents

Abstract

The present invention relates to a nanoemulsion emulsified cosmetic composition comprising nanocellulose and a method for producing the same. The particle size of the nanoemulsion of the present invention is small and homogeneous, thereby being excellent in skin penetration ability and having improved formulation stability. In addition, when the emulsified composition of the present invention is formulated as a cosmetic or external skin preparation, the delivery of active ingredients is improved, thereby producing a product having excellent effects.

Description

TECHNICAL FIELD The present invention relates to a nano-emulsion emulsion composition containing nano-cellulose and a method for producing the same,

The present invention relates to a cosmetic composition for emulsifying a nano emulsion using nanocellulose and a method for producing the same, and is characterized in that the particle size of the nanoemulsion of the present invention is small and homogeneous, excellent in skin penetration ability, and improved in formulation stability. In addition, the emulsified composition of the present invention can be used as cosmetics or external preparation for skin.

Cosmetics generally are formulated by combining ingredients that are not soluble in each other, such as water-soluble components and lipid-soluble components. In order to combine the above components, an emulsifier, that is, an emulsion, in which the two components are combined, is prepared using an emulsifier or a surfactant.

The size of the emulsion affects the stability of the phase and the ability to deliver effective substances. The smaller the size of the emulsion, the better the stability and the effective substance delivery capacity. The size of the emulsion can also influence phase stability in the formulation. Accordingly, as a method for solving such a problem, a nano-emulsified formulation having an emulsion particle size of several hundred nanometers has been developed. Various methods are known for preparing the nanoemulsion, but the methods using the high-pressure homogenizer and the method using the interfacial chemical properties, such as the phase-phase emulsification method and the D-phase emulsification method, are widely used. The method using the interfacial chemical properties is limited to use a limited emulsifier such as polyoxyethylene (POE) system. To date, ethylene oxide-added PEG-based compounds have been used as emulsifiers in the production of nanoemulsions. Recently, it has been reported that dioxins may be contained in the process of ethylene glycol polymerization, And there is a need for a way to avoid the use of emulsifiers which are of concern for irritation in accordance with the trends of recent consumers who value safety and wellbeing.

Compared to the interfacial chemical method, the high pressure homogenizer has the disadvantage of cost and place of the equipment and long time. However, the manufacturing method is free from the problems caused by the side effects and can be continuously manufactured.

In the present invention, a nanoemulsion was prepared using a high-pressure homogenizer, and nanocellulose was added thereto to reduce the size of the emulsion, thereby greatly increasing the human body transfer effect of the active material.

Korean Patent No. 10-1259452 Korean Patent Publication No. 10-2017-0103628

It is an object of the present invention to provide a nano-emulsion cosmetic composition containing nanocellulose particles.

Another object of the present invention is to provide a skin external preparation or cosmetic comprising a nano-emulsion emulsion composition containing nanocellulose particles.

In order to solve the above problems, the present invention provides a nano-emulsion emulsion composition comprising nanocellulose particles, wherein the nanocellulose particles are dispersed in the composition.

In one embodiment of the present invention, the nanocellulose particles are contained in an amount of 0.1 to 10% by weight based on the total weight of the composition.

In an embodiment of the present invention, the nanocellulose particles have an average size of 30 nm or less.

In one embodiment of the present invention, the nanocellulose may be selected from the group consisting of Kraft paper or sulfite pulp derived from various woods, powdered cellulose obtained by pulverizing them with a high-pressure homogenizer or mill, Microcrystalline cellulose powder purified by chemical treatment such as hydrolysis, bacterial-derived cellulose or kenaf, hemp, rice, bacas, bamboo, and the like can be used.

In one embodiment of the present invention, the nano emulsion has an average particle size of 8 to 30 nm, more preferably 12 to 18 nm.

In another aspect, the present invention provides a cosmetic comprising a nano-emulsion emulsion composition comprising nanocellulose particles.

In another aspect, the present invention provides an external preparation for skin comprising a nano-emulsion emulsion composition containing nanocellulose particles.

In another aspect, the present invention provides a method for producing a water-based ink composition comprising the steps of: (a) (b) adding an oily portion to the upper portion of the water, adding nano cellulose and stirring the mixture, and (c) homogenizing the composition of the step (b) at a high pressure to provide a nano emulsion cosmetic composition .

In one embodiment of the present invention, the high pressure homogenization step is performed at 300 to 800 psi, but is not limited thereto.

In another embodiment of the present invention, the high-pressure homogenization process is repeated 1 to 6 times, more preferably 4 to 5 times, but the present invention is not limited thereto.

The nano emulsion emulsion composition containing the nanocellulose particles of the present invention is characterized in that the particle size is smaller than that of the conventional nano emulsion and homogeneous and emulsification stability is secured compared with the conventional nano emulsion. Moreover, since the particle size is small, It has a feature that it can more effectively transfer the active ingredient into the skin.

FIG. 1 shows the results of measurement of particle size of nano-emulsion added with nanocellulose and visualization thereof.
Fig. 2 shows the results of measurement of particle size of nano-emulsion without added nanocellulose and visualization.
Figure 3 is a graph showing the content of skin moisture content when the nanoemulsion composition of the present invention contains a moisturizing active ingredient.
FIG. 4 is a graph showing a comparison of the degree of skin moisture content increase observed through FIG.

The present inventors have found that the size of the emulsion particle becomes smaller when the nanocellulose particles are contained in the formulation in order to make the size of the emulsion particle smaller and homogeneous in the emulsion composition of the nano emulsion formulation, Respectively.

That is, the present invention relates to an emulsion composition comprising a nanoemulsion, wherein the emulsion composition contains nanoshell particles dispersed in a particle state.

In the present invention, 'nanoemulsion' means an emulsion formulation in which a water phase and an oil phase are mixed, and the size of the emulsion particle ranges from several tens nm to several hundreds nm. When the size of the emulsified particles is larger than the skin lipid gaps, the effective ingredient contained in the composition is difficult to penetrate into the skin. Therefore, making the emulsified particles small is a very important technique in the formulation as in the present invention.

The nano-emulsion particle of the present invention is characterized by an average particle size of 8 to 30 nm, more preferably 12 to 18 nm. In one embodiment of the present invention, a nano emulsion having an average particle size of 16 nm was prepared. The conventional particle size in the conventional nanoemulsion formulation is generally in the range of several tens to several hundreds of nanometers, which limits the delivery of the active ingredient into the skin. The nanoemulsion of the present invention is characterized by being able to keep the particle size smaller by including nano-cellulose, and this property has further improved effect of penetrating the active ingredient into the skin.

As used herein, the term " average particle size " refers to the average diameter of particles in a liquid-liquid dispersion system, and since particles are three-dimensional objects, the particle size calculated using the concept of equivalent spheres . For example, an actual particle, such as a spherical shape having the same maximum length, a spherical shape having the same minimum length, a spherical shape having the same mass, a spherical shape having the same volume, a spherical shape having the same surface area, a spherical shape passing through the same sieve aperture, It is possible to calculate the particle size by the diameter of the equivalent particle in terms of the equivalent particle type having the same characteristics, and the average particle size can be regarded as an average value of the particle sizes of the particles. The average particle size includes the particle size measured by Dynamic Light Scattering (DLS). The dynamic light scattering method includes a method of determining the particle size by the Brownian motion of particles and includes a method of determining the particle size by reading the wavelength intensity of the scattered light (light) changing at a constant time interval. The light used in the method may include a laser. The equation for determining the particle size can be a commonly used one, and the equation also includes a Stoke-Einstein relation for the diffusion coefficient.

The 'emulsified' formulation is roughly divided into O / W (oil in water) emulsions in which the oil component is emulsified and a W / O (water in oil) emulsion in which the water component is emulsified in the oil component Recently, a W / O / W type emulsifier type in which a multi-liquid crystal film emulsification technique is introduced has been developed. The nanoemulsion emulsions of the present invention may include all of the above types, and more preferably, it may be a water-in-oil (W / O) formulation, but the present invention is not limited thereto.

The " nano-cellulose " of the present invention is a nano-sized cellulose-based raw material. The cellulose is obtained by crushing various types of wood-derived craft paper or sulfite pulp with a high-pressure homogenizer or mill Microcrystalline cellulose powder obtained by refining them by chemical treatment such as acid hydrolysis, cellulose derived from bacteria, and the like. In addition, plants such as kenaf, hemp, rice, bacchus and bamboo may also be used. In one embodiment of the present invention, cellulose derived from wood, especially pulp, cotton or bamboo, is used to produce nano-cellulose, but the present invention is not limited thereto.

The number average diameter of the 'nanocellulose' according to the present invention is 1 to 200 nm, preferably 1 to 150 nm, more preferably 1 to 100 nm, and most preferably 1 to 30 nm. In one embodiment of the present invention, the nanocellulose has a diameter of 20 nm or less. The nanocellulose may be in the form of a single microfibril or may be in the form of entangled nanofibers, but is not particularly limited. However, they are present in a form dispersed in the formulation.

The nanocellulose may be contained in the composition of the present invention in the form of a powder or an aqueous dispersion, more preferably in a water dispersed form. May be included in the total composition in an amount of 0.1 to 10% by weight, and more preferably in an amount of 1 to 5% by weight. When the amount of the nano-cellulose is less than 0.1% by weight, the effect on the particle size of the nano-emulsion is insignificant, and if it is more than 10% by weight, the properties of the composition may be affected. In one embodiment of the present invention, a nanoemulsion composition containing 3% by weight of the nanocellulose was prepared and its efficacy was evaluated.

In addition, the nanoemulsion emulsifying composition of the present invention may be contained in cosmetics, and the cosmetics may be prepared in any form conventionally produced in the art. For example, solutions, suspensions, emulsions, pastes, But are not limited to, gels, creams, lotions, powders, soaps, surfactant-containing cleansers, oils, powder foundations, emulsion foundations, wax foundations and sprays. More specifically, the present invention relates to a cosmetic lotion composition comprising a lotion, a cosmetic lotion, a nourishing lotion, a nutritive cream, a massage cream, a moisture cream, a moisture gel cream, a lotion, a gel, Packs, ointments, sticks, patches, sprays or powders.

In particular, the composition of the present invention can be included in functional cosmetics or general cosmetics. The term 'functional cosmetics' means that a professional therapeutic function of medicines is introduced into cosmetics, and unlike general cosmetics, the functional properties emphasizing physiologically active effects and effects For example, products that help skin to whiten, products that help to improve skin wrinkles, products that help skin to protect skin from UV rays, and cosmetics that are prescribed by the Health and Welfare Ordinance do. In one embodiment of the present invention, a cosmetic composition comprising a moisturizing active ingredient (hyaluronic acid) is prepared as an example, but the present invention is not limited thereto.

The composition of the present invention can be used in cosmetics as an adjuvant commonly used in cosmetics such as fatty substances, organic solvents, solubilizers, thickeners, gelling agents, softeners, antioxidants, suspending agents, stabilizers, surfactants, water, ionic or nonionic emulsifiers, fillers, sequestering agents, chelating agents, preservatives, vitamins, blocking agents, wetting agents, essential oils, dyes, pigments, hydrophilic or lipophilic active agents , Lipid vesicles, as well as any other ingredients conventionally used in cosmetics, as well as adjuvants commonly used in cosmetics or dermatology.

In another embodiment, the nanoemulsion emulsifying composition of the present invention can be used as an external preparation for skin. The term "external preparation for skin" is a concept that includes external products intended to be applied to the skin. Examples of the external use include those used for the purpose of treating, alleviating, treating or preventing diseases of human beings or animals, Refers to an article that does not act directly on the human body, is similar to a device or machine and similar, or is used for sterilization, insecticide and similar uses for the prevention of infection.

The external preparation for skin refers to a solid, semi-solid or liquid external medicine which can be easily applied to skin by mixing drugs with various bases such as oils, petrolatum, lanolin, and glycerol. External preparation formulations are not particularly limited, but may include, for example, powders, patches, gels, ointments, creams, liquids or aerosol formulations.

The present invention also provides a method for producing a nano-emulsion emulsion composition comprising nanocellulose particles,

(a) producing an upper water portion and an upper water portion; (b) adding an oily portion to the upper portion of the water, adding nano cellulose and stirring the mixture, and (c) homogenizing the composition of the step (b) at a high pressure to provide a nano emulsion cosmetic composition .

In the present invention, the step of high pressure homogenization after the addition of the aqueous phase, the oily phase and the nanocellulose is performed at a pressure of 300-800 psi. The pressure range is a condition in which the nanocellulose can be mixed homogeneously in the emulsified composition and emulsion particles can be produced in a nanoscale. The high-pressure homogenization is repeated one to six times, more preferably three to six times, though it is not limited thereto.

Hereinafter, the present invention will be described in more detail with reference to Examples. It will be apparent to those skilled in the art that these embodiments are merely illustrative of the present invention and that the scope of the present invention is not limited to these embodiments.

< Example >

Nano-cellulose  Particle-containing Nano emulsion  Preparation of composition

Emulsions were prepared with the compositions shown in Table 1 below. First, a water-soluble component, a moisturizer, and purified water are mixed and dissolved by heating (65-75 ° C) to prepare a water-soluble part. Then, the oil-soluble component, the emulsifier, and the oil are stirred and heated to dissolve to produce an oil-in-water portion. The emulsion composition of Example 1 was prepared by adding an oily portion to the upper part of the water and sufficiently stirring using a homomixer. The emulsion composition of Example 2 was prepared by treating it with a high pressure homogenizer.

The nanoemulsion composition of Example 3 was prepared by adding 3% by weight of nano-cellulose having a diameter of 20 nm or less to the emulsion of Example 1, and the same was passed through a high-pressure homogenizer to prepare the nanoemulsion composition of Example 4. The high-pressure homogenizer was treated at 300 to 800 psi for 4 to 5 times, and the same procedure was applied to all the examples.

name Example 1 (% by weight) Example 3
(weight%) One Purified water to 100 to 100 2 Nano-cellulose 0 3.0 Hyaluronic acid 1% 2.0 2.0 2 Glycerine 5.0 5.0 4 Glycereth-26 2.0 2.0 5 Carbomer 941 (25%)
(sodium polyacrylate 941) 10.0 10.0 6 Phenoxyethanol 0.4 0.4 7 Triethanolamine (TRIETHANOL AMINE) 0.5 0.5 8 Coconut oil 0.05 0.05 9 Polyoxyethylene (5) Oleyl Ether 1.0 1.0 Total amount 100 100

The particle size analysis of the nano-emulsion and the nano-emulsion added with nanocellulose prepared as described above was carried out. The particle size analyzer used was a Dynamic Light Scattering Spectrophotometer (DLS-7000, Otsuka Electronics, Japan) Respectively.

As a result, as shown in FIG. 1, in the case of the nano-emulsion in which the nanocellulose was added, the particle size was in the range of 8 to 30 nm and the average particle size was measured to be 16 nm. In the case of the nano- And a particle size of 65 to 300 nm.

That is, in the case of the nano-emulsion containing nanocellulose, the particle size and homogeneity of the emulsion became very high.

<Experimental Example>

Evaluation of Moisturizing Ability of Cosmetic Composition Containing Nano Emulsion

(1) Evaluation of skin moisture content

In order to evaluate the skin-transferring power of the nano-emulsion containing nanocellulose prepared in the above example, an experiment was conducted to measure the transdermal delivery rate of the skin moisturizing component. The emulsions of Examples 1 to 4 were applied for two weeks in the morning and evening on the inner part of the humpback for women aged 18 to 55 years old. After 1 week (1 W), 2 weeks After each week (2 W), skin moisture content was measured. To reduce the measurement error, each test was performed by the same test person. The skin test was performed after the skin was stabilized for at least 30 minutes under constant temperature and humidity conditions (23 ± 1 ° C, 50 ± 2% RH) Respectively.

Skin moisture content was measured using Skin-O-Mat® (Cosmomed inc, Germany). Measurements are expressed as a value between 0.0 and 125.0 (AU: arbitrary unit). The higher the moisture content of the skin, the higher the measured value. In this experiment, the skin surface at the same position was repeatedly measured three times at each measurement period, and the average value thereof was evaluated.

The measured values for the degree of skin moisture content are shown in Table 2 and FIG. In the case of the general nano emulsion, the degree of water content was slightly increased for two weeks. However, in the case of the nano-emulsion containing nanocellulose as in Example 3 and Example 4, the degree of water content after 2 weeks was remarkably I can confirm that it is improved.

0 Week 1 Week 2 Week Example 1 25.1 ± 5.73 31.0 + 4.81 ^a 32.8 ± 5.30 ^a Example 2 26.1 ± 6.14 34.0 ± 3.15 ^ab 33.1 ± 4.52 ^a Example 3 27.0 + - 6.49 34.9 ± 3.91 ^ab 36.1 ± 3.93 ^ae Example 4 26.7 ± 6.78 37.6 ± 2.98 ^abcd 39.2 + 4.29 ^aef

a: 0w vs.. 1 w, 2 w, ANOVA, significant: p < 0.05

b: 1 w, Example 1 vs. Example 2, Example 3, Example 4, ANOVA, significant: p < 0.05

c: 1 w, Example 2 vs. Example 4, ANOVA, significant: p < 0.05

d: 1 w, Example 3 vs. Example 4, ANOVA, significant: p < 0.05

e: 2 w, Example 1 vs. Example 3, Example 4, ANOVA, significant: p < 0.05

f: 2 w, Example 2 vs. Example 4, ANOVA, significant: p < 0.05

(2) Moisture content of skin  Rate of Change % ) evaluation

Skin-O-Mat® (Cosmomed inc, Germany) data was used to calculate the percent change in skin moisture content over time. Compared with before use, the rate of change in skin moisture content after 1 week of use and 2 weeks after use was compared and evaluated. The rate of increase or decrease in skin moisture content was calculated using the following equation.

All measurements were repeated three times and the average value was obtained. The statistical analysis was confirmed by the 95% confidence interval, and the validity of the results was tested by the Kolmogorov-Smirnov and Shapiro-Wilk methods. One-way ANOVA was used to analyze changes in skin moisture content and skin moisture content before and after use. Statistical analysis program was SPSS 23.0 (IBM SPSS Statistics, USA).

The rate of increase or decrease in the skin moisture content measured as described above is shown in Table 3 and FIG. In the case of the nano-emulsion containing the nanocellulose of the present invention (Examples 3 and 4), it was confirmed that the rate of increase of the skin moisture content was higher than that of the general nano-emulsion.

1 week 2 week Example 1 28.2 ± 7.59 35.5 ± 11.08 Example 2 35.5 ± 7.72 30.4 ± 7.32 Example 3 33.3 ± 5.30 36.9 ± 5.83 Example 4 46.8 ± 7.16 51.4 ± 8.16

The present invention has been described with reference to the preferred embodiments. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims. Therefore, the disclosed embodiments should be considered in an illustrative rather than a restrictive sense. The scope of the present invention is defined by the appended claims rather than by the foregoing description, and all differences within the scope of equivalents thereof should be construed as being included in the present invention.

Claims (12)

A nano emulsion cosmetic composition comprising nanocellulose particles. The method according to claim 1,
Wherein the nanocellulose particles are dispersed in the composition. The method according to claim 1,
Wherein the nanocellulose particles are contained in an amount of 0.1 to 10% by weight based on the total weight of the composition. The method according to claim 1,
Wherein the nanocellulose particles have an average size of 30 nm or less. The method according to claim 1,
The nano-cellulose may be powdered cellulose obtained by crushing various kinds of wood-derived craft paper or sulfite pulp, a high-pressure homogenizer or a mill, or a chemical treatment such as acid hydrolysis Microcrystalline cellulose powder, bacterial-derived cellulose or kenaf, hemp, rice, bacas, bamboo, and the like. The method according to claim 1,
Wherein the nano-emulsion particles have an average particle size of 8 to 30 nm. 7. The method according to any one of claims 1 to 6,
Wherein the cosmetic composition is for skin moisturizing. An external preparation for skin comprising a nano-emulsion containing nanocellulose particles. 9. The method of claim 8,
Wherein the external preparation for skin is at least one selected from powder, patch, gel, ointment, cream, liquid or aerosol. (a) producing an upper water portion and an upper water portion;
(b) adding an oil-in-water portion to the upper portion of the water, adding nano-cellulose and stirring the mixture, and
(c) homogenizing the composition of step (b) at a high pressure to prepare a nano-emulsion cosmetic composition. 11. The method of claim 10, wherein the intimate homogeneous is performed at a pressure of 300-800 psi. The method of manufacturing a nano emulsion cosmetic composition according to claim 10, wherein the step of homogenizing the high pressure is repeated 3 to 6 times.

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