KR102566764B1 - Composition for moisturizing, mask-pack, cosmetics, and method for preparation thereof - Google Patents

Abstract

The present specification provides a moisturizing composition containing carboxymethylated cellulose and hyaluronic acid and having a viscosity of 600 to 750 cP at 25° C., a mask pack containing the moisturizing composition, cosmetics, and a manufacturing method thereof.

Description

Moisturizing composition, mask pack, cosmetics and manufacturing method thereof

The present specification relates to a moisturizing composition and a method for preparing the same.

When the skin moisturizing function is lowered, aging of the skin is accelerated, resulting in skin damage and skin diseases. In order to maintain the moisture of the skin due to the deterioration of the moisturizing function, various cosmetics capable of supplying moisture or preventing moisture loss have been developed.

Among them, hyaluronic acid used as a moisturizer is widely used in the field of cosmetics because of its good feeling of use and excellent moisturizing ability. However, it is difficult to mix with other substances due to its very high viscosity, and is used in small amounts because it is expensive.

On the other hand, because of the excellent physical properties of nano-sized materials, interest in making nanocomposite materials is greatly increasing worldwide. In particular, cellulose is the most abundant polymer material obtained from nature and has many advantages such as excellent mechanical strength and biodegradability. Nanocellulose can be used in various fields due to its excellent physical properties and transparent optical properties, and has recently been attracting attention as a material that is in the spotlight in the beauty field.

Korean Patent Publication No. 10-2014-0113615

The present specification is intended to provide a moisturizing composition and a manufacturing method thereof.

An exemplary embodiment of the present specification provides a moisturizing composition including carboxymethylated cellulose nanofibers and hyaluronic acid, and having a viscosity of 600 to 750 cP at 25 °C.

Another embodiment of the present specification provides a mask pack containing the above-described moisturizing composition as a lotion.

One embodiment of the present specification provides a cosmetic comprising the aforementioned moisturizing composition.

An exemplary embodiment of the present specification includes preparing carboxymethylated cellulose by modifying cellulose fibers; Nanonizing the carboxymethylated cellulose; And it provides a method for preparing the above-described moisturizing composition comprising the step of preparing the above-described moisturizing composition comprising carboxymethylated cellulose nanofibers and hyaluronic acid.

The moisturizing composition of the present invention has a lower viscosity than hyaluronic acid, making it easy to mix with other additives that may be included in cosmetics, and having a higher viscosity than non-nanoized carboxymethylated cellulose aqueous solution, it is suitable for use as a cosmetic such as a moisturizer, and has excellent thickening. can have an effect. In addition, since the moisture content is high, the moisturizing effect is excellent, and the price is cheaper than using hyaluronic acid alone, there is an advantage in the process that mass production is possible in an economical way.

1 is a graph showing the moisture retention rate over time of the moisturizing compositions according to Examples 1 to 3.
Figure 2 is a graph showing the water retention rate over time of the compositions according to Example 1 and Comparative Examples 1 and 2.
Figure 3 is a graph showing the moisture retention rate over time of the compositions according to Example 1 and Comparative Examples 3 and 4.

Hereinafter, the present invention will be described in detail.

In this specification, when a part is said to "include" a certain component, it means that it may further include other components without excluding other components unless otherwise stated.

An exemplary embodiment of the present specification provides a moisturizing composition including carboxymethylated cellulose nanofibers and hyaluronic acid, and having a viscosity of 600 to 750 cP at 25 °C.

Cellulose nanofibers mean that they are nanonized by applying shear force after removing hemicellulose and lignin from wood pulp, which is a raw material. Cellulose nanofibers also have a high crystallinity of 40 to 90%, and are characterized by excellent physical properties due to high thermal stability, mechanical strength, and elastic modulus. Cellulose nanofibers can be prepared by dispersing the pulp in water and then mechanically treating it using a grinder or a homogenizer, which is a high-pressure homogenizer. The most used equipment in small units is the grinder, and the most commercialized equipment is the homogenizer, which is a high-pressure homogenizer. When using the above equipment, a physical force such as shear force, frictional force, or impact force is applied to the cellulose fibers to nanonize the pulp. Through this, an aqueous solution in which cellulose nanofibers are 1 to 5 parts by weight based on 100 parts by weight of the total aqueous solution containing cellulose nanofibers is prepared. Nanoization of pulp may mean fibrillation.

In the present specification, the diameter of the cellulose nanofibers included in the cellulose nanofibers may be 10 to 60 nm, specifically 10 to 30 nm. If the diameter of the cellulose nanofibers is less than 10 nm, physical properties of the film may be reduced, and if the diameter is greater than 60 nm, bonding strength between the cellulose nanofibers may be reduced.

In addition, in the present specification, the length of the cellulose nanofibers may be 100 nm to 10 μm, specifically 1 to 5 μm. If the length of the cellulose nanofibers is less than 100 nm, physical properties of the film may be reduced, and if the length is greater than 10 μm, the bonding force between the cellulose nanofibers may be reduced.

In one embodiment of the present specification, the cellulose nanofibers are carboxymethylated. Carboxymethylation means substituting a hydroxy group (celluose-OH) substituted at C6 of a glucose residue constituting cellulose with a carboxymethyl group (-CH ₂ COOH) (celluose-O-CH ₂ COOH). Transparency can be secured by carboxymethylation of the cellulose nanofibers. In addition, since the carboxymethyl group introduced into the cellulose nanofibers is hydrophilic, and hydrogen bonds between the carboxymethyl groups or with the hydroxyl groups included in the cellulose nanofibers are possible, the water content can be further increased.

Hyaluronic acid is a biopolymer material, and is widely used for medical and medical devices and cosmetics due to its excellent biocompatibility and viscoelasticity. In the present specification, hyaluronic acid is used as a meaning including all of hyaluronic acid itself, salts thereof, or combinations thereof. The salt of hyaluronic acid may include both inorganic salts such as sodium hyaluronate, potassium hyaluronate, calcium hyaluronate, magnesium hyaluronate, zinc hyaluronate and cobalt hyaluronate, and organic salts such as tetrabutylammonium hyaluronate. The molecular weight of the hyaluronic acid may be 100,000 to 5,000,000.

One embodiment of the present specification provides a moisturizing composition having a viscosity of 600 to 750 cP at 25 °C. In another exemplary embodiment, the viscosity may be 610 to 710 cP. When the viscosity of the moisturizing composition of the present invention satisfies the above range, it can be easily mixed with other additives and has an excellent moisture content, so that it can be effectively used as a cosmetic such as a moisturizer. Specifically, when the viscosity is less than 600 cP, the viscosity is too low and easily flows down when applied to the skin, and it is difficult to control when used as a cosmetic such as a moisturizer, and both the thickening effect and moisturizing effect may be reduced. When the viscosity is greater than 750 cP, mixing with other additives is difficult because the viscosity is too high.

The range of the viscosity may be adjusted according to the content of the carboxymethylated cellulose nanofibers and hyaluronic acid. In addition, it may be adjusted according to the degree of modification or nanoization of the carboxymethylated cellulose nanofibers.

Specifically, the degree of modification of the carboxymethylated cellulose nanofibers can be determined according to the carboxymethyl group content. In one embodiment of the present specification, the carboxymethyl group content may be 480 to 580 μmol / g, preferably 510 to 540 μmol / g based on the total dry amount of carboxymethylated cellulose nanofibers.

The carboxymethyl group content can be measured by a method described later. Prepare a mixture of 200 g in total, including 0.6 g of carboxymethylated cellulose nanofibers, 2 ml of 0.1 M sodium chloride solution (NaCl, sodium chloride solution), and deionized water in a 250 mL beaker. Insert a magnetic bar into the beaker, and insert the pH meter and conductivity meter into the beaker using a stand so that they do not touch the magnetic bar. While stirring the mixture, 0.1M hydrochloric acid (HCl) was added to adjust the pH to 3. At this time, when a large amount of hydrochloric acid is added at once, aggregation between carboxymethylated cellulose nanofibers may occur, so it is added dropwise.

Thereafter, 0.5 mL of 0.05 M sodium hydroxide solution (NaOH, sodium hydroxide solution) was added to the pH 3 mixture containing the carboxymethylated cellulose nanofibers, stirred for 10 seconds, and then the conductivity was recorded.

When the conductivity reaches phase 3, where the conductivity rapidly increases after passing a certain period, the titration is terminated. At least, titration is performed until the conductivity reaches the conductivity (y value when x = 0) at the point where the pH of the mixture is 3.

Draw a graph with the amount of sodium hydroxide (NaOH) added as the X-axis (mL) and the conductivity (μS/cm) as the Y-axis. The linear trend line (linear equation) of each period is obtained by dividing the conductivity into a period in which the conductivity rapidly decreases (phase 1), a period in which the conductivity is maintained (phase 2), and a period in which the conductivity rapidly rises (phase 3).

The intersection of the phase 1 trend line and the phase 2 trend line and the intersection of the phase 2 and phase 3 trend lines are obtained, and the X values of the intersections are set to V1 and V2, respectively, and then the carboxymethyl group content is calculated through Equation 1 below.

[Calculation 1]

In Equation 1, CNaOH is the concentration of sodium hydroxide (mol·L ^-1 ), Mcnf is the total dry amount of carboxymethylated cellulose nanofibers (kg), and V1 and V2 are as described above.

In addition, the degree of nanoization of the carboxymethylated cellulose nanofibers can be determined according to the diameter size of the carboxymethylated cellulose nanofibers. The diameter of the carboxymethylated cellulose is preferably 10 to 60 nm, and specifically may be 10 to 30 nm.

The diameter of the carboxymethylated cellulose nanofibers can be measured using a scanning electron microscope (SEM) equipment, and can be expressed by calculating the average value of the measured values several times. The SEM equipment may be, for example, HITACHI's scanning electron microscope S-4800, but is not limited thereto.

In one embodiment of the present specification, the carboxymethylated cellulose nanofibers have a carboxymethyl group content of 480 to 580 μmol / g and a diameter of 10 to 30 nm, so that the viscosity of the moisturizing composition of the present invention has a viscosity of 600 to 750 cP A moisturizing composition may be provided.

On the other hand, the composition containing non-nanoized carboxymethylated cellulose (CMC) and hyaluronic acid has a viscosity of 450 to 460 cP, which is lower than that of the moisturizing composition of the present invention. This is because, unlike the carboxymethylated cellulose nanofibers of the present invention, the carboxymethylated cellulose fibers do not go through a nano-nanoization process, and thus the exposure of hydrophilic groups such as hydroxyl groups (-OH) to the surface is small.

In the present invention, the viscosity of the moisturizing composition may be measured at 25° C., 30 seconds or 60 seconds under the condition of 75 spindle, 50 RPM using a Brookfield viscometer.

In the present invention, the moisturizing composition has a moisture retention rate of 7% or more at a drying temperature of 32° C., a relative humidity of 25%, and drying for 4 hours. In another exemplary embodiment, the water retention rate of the moisturizing composition is 7% or more and 100% or less, preferably 7% or more and 20% or less. In another exemplary embodiment, the moisturizing composition has a moisture retention rate of 20% or more, specifically 21% or more and 100% or less at a drying temperature of 32° C., a relative humidity of 25%, and drying for 3 hours. In another embodiment, the moisturizing composition has a moisture retention rate of 0.7% or more, specifically 0.7% or more and 100% or less at a drying temperature of 32 ° C., a relative humidity of 25%, and drying for 5 hours.

In addition, since the moisture retention time of the moisturizing composition is 0 to 15 hours, it is possible to supply moisture to the skin for a sufficient time. By satisfying the water retention rate and water retention time within the above ranges, the moisturizing composition can be suitably used for cosmetics for supplying moisture, such as a moisturizer.

The water retention rate is measured by a method described later. A filter paper is placed on a Petridish, and a moisturizing composition according to an exemplary embodiment of the present invention is placed thereon. The weight of the composition is measured at a drying temperature of 32° C. and a relative humidity of 25% at regular time intervals until no change in weight is seen, and the water retention rate is calculated by the following formula 2.

[Calculation 2]

In Equation 2, the constant time may mean 4 hours. In another exemplary embodiment, the predetermined time may mean 3 hours. In addition, the predetermined time may mean 5 hours. In another exemplary embodiment, the predetermined time may mean 30 minutes, 1 hour, 2 hours, 6 hours, or 15 hours.

In one embodiment of the present specification, the moisturizing composition has a carboxymethylated cellulose nanofiber content of 0.1 to 5% by weight, based on 100% by weight of the moisturizing composition, and a hyaluronic acid content of 0.1 to 5% by weight based on 100% by weight of the moisturizing composition. am. When the content of carboxymethylated cellulose nanofibers and hyaluronic acid satisfies the above range, the composition of the present invention may have appropriate viscosity and water retention rate for use in cosmetics such as a moisturizer.

In one embodiment of the present specification, the content of the carboxymethylated cellulose nanofibers and hyaluronic acid in the moisturizing composition may be 0.2 to 1% by weight relative to 100% by weight of the moisturizing composition. Preferably it may be 0.2 to 0.8% by weight. By satisfying the above range, the moisturizing composition of the present invention may have appropriate viscosity and water retention rate for use as a cosmetic such as a moisturizer.

In one embodiment of the present specification, the moisturizing composition may further include distilled water. The distilled water may be 90 to 99.8% by weight relative to 100% by weight of the moisturizing composition. In another exemplary embodiment, the distilled water may be 99 to 99.8% by weight relative to 100% by weight of the moisturizing composition. Preferably it may be 99.2 to 99.8% by weight.

An exemplary embodiment of the present specification provides a moisturizing composition in which the mixing ratio of the carboxymethylated cellulose nanofibers and the hyaluronic acid is 3:7 to 7:3. The ratio may be 3:7, 5:5 or 7:3. Preferably, the mixing ratio of the carboxymethylated cellulose nanofibers and the hyaluronic acid may be 7:3. When the mixing ratio satisfies the range of 3:7 to 7:3, the composition of the present invention may have appropriate viscosity and moisture retention for use in cosmetics such as a moisturizer.

Specifically, the higher the ratio of carboxymethyl cellulose nanofibers to that of hyaluronic acid, the higher the water retention rate of the moisturizing composition. This is because the negatively charged carboxymethyl cellulose nanofibers tend to agglomerate with each other, and when the negatively charged hyaluronic acid is mixed, the hyaluronic acid acts as a dispersing agent, resulting in improved water retention performance. Excellent carboxymethyl cellulose nanofibers can be dispersed. Thus, by including a large amount of the carboxymethyl cellulose nanofibers in which the moisturizing composition is dispersed, the water retention rate may be further increased.

In one embodiment of the present invention, the above-described moisturizing composition may be included in a mask pack as a lotion. A mask pack is used to supply nutrients and moisture to the face. In general, after impregnating a base material such as non-woven fabric with cosmetic ingredients such as toner, and attaching the mask pack to the skin so that the cosmetic ingredients can be delivered to the skin. It is widely used for removing after a certain period of time. In addition, the mask pack can be used not only for the face but also for the whole body other than for the neck, shoulders, arms, and legs, and cosmetic ingredients such as the lotion may include water and surfactants, thickeners, preservatives, fragrances, or oils. In addition, it is not particularly limited as long as it improves skin beauty functions such as moisture supply, whitening, anti-aging, lifting, and soothing in the related art.

In the present specification, the mask pack may further include a support. Nonwoven fabric, hydrogel, or biocellulose may be used as the support, but it is not particularly limited as long as it is used as a support for mask packs in the art.

In the present invention, the shape of the mask pack may be manufactured in various shapes according to the skin attachment area. In general, the shape of the mask pack is manufactured according to the shape of the face with holes for the eyes and mouth. In addition, there may be mask packs dedicated to the eyes, nose, and lips, and the shape is not particularly limited. In addition, the mask pack may have a planar structure or a three-dimensional structure.

In one embodiment of the present specification, the aforementioned moisturizing composition may be included in cosmetics. The cosmetics may further include additives as needed. As an additive, glycerin, collagen, 1,3-butylene glycol, or sodium-pyrrolidonecarboxylic acid may be further included, but is not limited thereto, and as long as it improves skin moisturizing function, it may be further included without being particularly limited. .

In another exemplary embodiment, the cosmetics including the moisturizing composition may further include a functional material capable of enhancing skin care effects.

According to another exemplary embodiment, the moisturizing composition can be used as a peel off mask that can be spread on the face without a separate support such as nonwoven fabric.

By including hyaluronic acid in the moisturizing composition, it is possible to prepare a composition with good skin feel. When hyaluronic acid is used alone, it is difficult to mix it with other additives that may be included in cosmetics due to its high viscosity. In addition, since hyaluronic acid is expensive, it may be uneconomical to use in large quantities. However, by including the carboxymethylated cellulose nanofibers and hyaluronic acid in the moisturizing composition according to the present invention, the viscosity is lower than that of hyaluronic acid alone, so it is easy to mix other additives. In addition, it is economical because the price is lower than that of using hyaluronic acid alone, and the moisturizing effect is superior because the water retention rate of the composition is high.

An exemplary embodiment of the present specification includes preparing carboxymethylated cellulose by modifying cellulose fibers; Nanonizing the carboxymethylated cellulose; And it provides a method for preparing a moisturizing composition comprising the step of preparing a moisturizing composition comprising carboxymethylated cellulose nanofibers and hyaluronic acid.

In one embodiment of the present specification, preparing carboxymethylated cellulose by modifying the cellulose fibers may include dispersing the cellulose fibers in alcohol. The alcohol may be isopropyl alcohol (IPA).

Thereafter, a step of stirring the solution in which the cellulose fibers are dispersed in alcohol into an alkaline solution may be further included. The alkali solution may be a sodium hydroxide (NaOH) solution and may further include alcohol. The alcohol may be isopropyl alcohol (IPA).

In addition, after adding monochloroacetic acid, a carboxymethylation reaction may be performed by heating. Thereafter, a step of washing the carboxymethylated cellulose fibers produced by the carboxymethylation reaction may be further included. The washing step may be performed with distilled water using a suction filtration method or a centrifugal separation method, and preferably, a suction filtration method may be used.

The suction filtration method means a method of increasing the filtration rate by lowering the pressure on the lower surface than the pressure on the surface of the liquid during filtration. The centrifugal separation method refers to using a density difference between a solid and a liquid surrounding the solid by applying a centrifugal force by rotating a material around an axis.

As a method that can be applied in the step of preparing carboxymethylated cellulose by modifying cellulose fibers, a method of hydrolyzing cellulose fibers with an acid or an enzyme, a TEMPO-medicated oxidation method, or an alkali solution and monochloroacetic acid There is a carboxymethylation reaction used.

In the present invention, carboxymethylated cellulose can be prepared by a carboxymethylation reaction using an alkali solution and monochloroacetic acid. Specifically, the alkali solution may be a sodium hydroxide (NaOH) solution, and may further include alcohol as needed. The alcohol may be isopropyl alcohol (IPA).

The step of nanonizing the modified cellulose fibers, carboxymethylated cellulose, means a process of dispersing the aggregated cellulose fibers in water and then physically pulverizing them using a grinder or a homogenizer, which is a high-pressure homogenizer. do.

In one embodiment of the present specification, modified carboxymethylated cellulose may be nanonized using a grinder. Specifically, the grinder may be a commercially available Masko grinder.

By undergoing a process of nanonizing carboxymethylated cellulose using a grinder or homogenizer, a hydrophilic functional group such as a hydroxyl group or a carboxymethyl group included in cellulose may be further exposed to the surface. The exposed hydroxyl group or carboxymethyl group may form a hydrogen bond with each other or each, and when the moisturizing composition of the present invention is produced in a process in which water is used, the physical properties of the composition may not be easily modified. Accordingly, mass production is possible, and the efficiency of the production process can be increased.

Unlike the moisturizing composition of the present invention containing carboxymethylated cellulose nanofibers, when the composition containing carboxymethylated cellulose is electrostatically spun to produce nanofibers, the spun nanofibers are produced by electrostatic force. As such, when other additives or functional substances that may be included in cosmetics are included, the composition may not be well mixed. In addition, when a liquid composition is nanonized by an electrostatic spinning method, it is dried or cured and solidified. Accordingly, it is impossible to measure the viscosity of the solidified composition. The electrostatic spinning method is a method of producing micro- or nano-sized fibers by applying a high voltage to a polymer solution, and means that the prepared nano-sized fibers are composed of a polymer. On the other hand, the carboxymethylated cellulose nanofibers prepared by mechanically converting the carboxymethylated cellulose of the present invention into nanoparticles include nanoparticles with a high aspect ratio composed of polymers. When carboxymethylated cellulose is manufactured into nanofibers by a mechanical method, since the nanofibers exist in a dispersed state in an aqueous solution, there is an advantage in that they can be easily mixed with other additives or functional substances that may be included in cosmetics. In addition, the carboxymethylated cellulose nanofibers of the present invention have a smaller diameter than nanofibers prepared by electrostatic spinning, have excellent mechanical properties, and are more suitable for mass production.

In the step of preparing the moisturizing composition comprising the carboxymethylated cellulose nanofibers and hyaluronic acid, the above-described moisturizing composition may be prepared by mixing the carboxymethylated cellulose nanofibers and hyaluronic acid in a ratio of 3: 7 to 7: 3 . In addition, the moisturizing composition may be prepared by further including distilled water if necessary. The moisturizing composition may be prepared by stirring using an impeller.

Hereinafter, examples will be described in detail in order to specifically describe the present specification. However, embodiments according to the present specification may be modified in many different forms, and the scope of the present specification is not construed as being limited to the embodiments described below. The embodiments herein are provided to more completely explain the present specification to those skilled in the art.

Example .

1. Preparation of Moisturizing Composition

( carboxymethylation Preparation of Cellulose Nanofibers)

A pulp stock was prepared by dispersing 45 g (whole dry weight) of cellulose fibers in 1.5 L of isopropyl alcohol (IPA).

Then, 7.2 g of sodium hydroxide (NaOH) was added to 2.5 L of isopropyl alcohol (IPA), stirred at 40 for 30 minutes, and then 1,600 g of the dispersed pulp stock was added and stirred for 30 minutes to prepare a solution.

Thereafter, 4.5 g of dissociated chloroacetic acid was added to 500 ml of the solution, followed by heating at 5 and reacting for 3 hours. After the reaction, the solution was washed with distilled water using a suction filtration method.

The solution after washing was dispersed in distilled water at 1% by weight based on the total weight of the entire solution, and then applied repeatedly 7 to 10 times at 1500 RPM with Masko grinder stone spacing 40 μm to prepare carboxymethylated cellulose nanofibers did

( carboxymethylation of cellulose nanofibers carboxymethyl group content and diameter measurement)

The carboxymethyl group content of the prepared carboxymethylated cellulose nanofibers was measured by the method described below.

Carboxymethylated cellulose nanofibers were prepared in a 250mL beaker to make a total mixture of 200g, including 0.6g of the dry amount, 2ml of 0.1M sodium chloride solution (NaCl, sodium chloride solution), and deionized water.

A magnetic bar was placed in the beaker, and the pH meter and the conductivity meter were inserted into the beaker using a stand so that they do not touch the magnetic bar. While stirring the mixture, 0.1M hydrochloric acid (HCl) was added to adjust the pH to 3. At this time, when a large amount of hydrochloric acid is added at once, aggregation between carboxymethylated cellulose nanofibers may occur, so it was added dropwise.

0.5 mL of 0.05 M sodium hydroxide solution (NaOH, sodium hydroxide solution) was added to the pH 3 mixture containing the carboxymethylated cellulose nanofibers, stirred for 10 seconds, and then conductivity was recorded.

The titration was terminated when the conductivity reached phase 3, where the conductivity rapidly increased after passing a certain period. Titration was carried out until at least the conductivity reached the point where the pH of the mixture was 3 (y value when x = 0).

A graph was drawn with the amount of sodium hydroxide (NaOH) added as the X-axis (mL) and the conductivity (μS/cm) as the Y-axis. A linear trend line (straight line equation) was obtained for each period by dividing the conductivity into a period in which the conductivity rapidly decreased (phase 1), a period where the conductivity was maintained (phase 2), and a period where the conductivity rapidly increased (phase 3).

The intersection of the phase 1 trend line and the phase 2 trend line and the intersection of the phase 2 and phase 3 trend lines were obtained, and the X values of the intersection were set to V1 and V2, respectively, and then the carboxymethyl group content was calculated through Equation 1 below.

[Calculation 1]

In Equation 1, CNaOH is the concentration of sodium hydroxide (mol·L ^-1 ), Mcnf is the total dry amount of carboxymethylated cellulose nanofibers (kg), and V1 and V2 are as described above. As a result of measuring the carboxymethyl group content by the above method, it was 530 μmol/g.

In addition, the diameter of the prepared carboxymethylated cellulose nanofibers was measured using HITACHI's scanning electron microscope S-4800 model, and the value was 10 to 30 nm.

( carboxymethylation Preparation of Moisturizing Composition Containing Cellulose Nanofibers and Hyaluronic Acid)

Example 1-moisturizing composition 1

10 g of a mixture was prepared by using carboxymethylated cellulose nanofibers and hyaluronic acid at a ratio of 7:3. Thereafter, 10 g of a moisturizing composition was prepared by using 0.5% by weight of the mixture and 99.5% by weight of distilled water based on 100% by weight of the moisturizing composition.

Thereafter, the moisturizing composition 1 was prepared by stirring at 500 RPM for 10 minutes using an impeller.

Example 2-moisturizing composition 2

Moisturizing composition 2 was prepared in the same manner as in Example 1, except that 10 g of a mixture was prepared using carboxymethylated cellulose nanofibers and hyaluronic acid at a ratio of 5:5.

Example 3-moisturizing composition 3

Moisturizing composition 3 was prepared in the same manner as in Example 1, except that 10 g of a mixture was prepared by using carboxymethylated cellulose nanofibers and hyaluronic acid in a ratio of 3:7.

2. Viscosity measurement

Moisturizing compositions 1 to 3 prepared in Examples 1 to 3 were measured for each viscosity at 75 spindle, 50RPM, 25 ° C., 30 seconds and 60 seconds using a Brookfield viscometer. The measured viscosities are listed in Table 1 below.

3. Measurement of water retention

After placing filter paper on a Petridish, a moisturizing composition was placed thereon. Thereafter, the weight of the Petri dish on which the moisturizing compositions 1 to 3 were placed was measured at a drying temperature of 32 ° C. and a relative humidity of 25% for 30 minutes, 1, 2, 3, 4, 5, 6, and 15 hours. Then, after calculating the water retention rate by the following formula 2, the values are shown in Table 2 below.

[Calculation 2]

In Equation 2, the constant time means 30 minutes, 1, 2, 3, 4, 5, 6 or 15 hours.

comparative example One.

10 g of an aqueous solution containing carboxymethylated cellulose nanofibers alone was prepared. The carboxymethylated cellulose nanofibers were included in 0.5% by weight compared to 100% by weight of the aqueous solution. Viscosity and water retention were measured in the same manner as described in the above examples with the prepared aqueous solution, and are shown in Tables 1 and 2 below.

comparative example 2.

10 g of an aqueous solution containing hyaluronic acid alone was prepared. The hyaluronic acid was included in 0.5% by weight relative to 100% by weight of the aqueous solution. Viscosity and water retention were measured in the same manner as described in the above examples with the prepared aqueous solution, and the values are shown in Tables 1 and 2 below.

comparative example 3.

10 g of an aqueous solution containing unnanoized carboxymethylated cellulose and hyaluronic acid was prepared. The carboxymethylated cellulose was included at 0.25% by weight based on 100% by weight of the aqueous solution, and the hyaluronic acid was included at 0.25% by weight based on 100% by weight of the aqueous solution. Viscosity and water retention were measured in the same manner as described in the above examples with the prepared aqueous solution, and are shown in Tables 1 and 2 below.

comparative example 4.

10 g of an aqueous solution containing only non-nanoized carboxymethylated cellulose was prepared. The carboxymethylated cellulose was included in an amount of 0.5% by weight based on 100% by weight of the aqueous solution. Viscosity and water retention were measured in the same manner as described in the above examples with the prepared aqueous solution, and are shown in Tables 1 and 2 below.

Components of the composition (ratio of components) Viscosity at 30 seconds (cP) Viscosity at 60 seconds (cP) Example One CM-CNF+HA (CM-CNF:HA=7:3) 644.9 640.9 Example 2 CM-CNF+HA (CM-CNF:HA=5:5) 623 623 Example 3 CM-CNF+HA (CM-CNF:HA=3:7) 708.8 700.8 comparative example One CM-CNF 1162 1182 comparative example 2 HA 942.5 946.5 comparative example 3 CMC+HA 455.3 451.3 comparative example 4 CMC - -

In the components of the composition of Table 1, CM-CNF means carboxymethylated cellulose nanofiber, HA means hyaluronic acid, and CMC means carboxymethylated cellulose that is not nano-sized, respectively.

In Table 1, the composition containing only carboxymethylated cellulose (CMC) (Comparative Example 4) had too low viscosity and could not be measured with a viscometer.

According to Table 1, it was confirmed that the viscosity of the moisturizing compositions of Examples 1 to 3 was higher than that of Comparative Example 3.

On the other hand, it was found that Comparative Examples 1 and 2 had 300 cP or more higher viscosity than Examples 1 to 3. This confirmed that mixing with other additives that may be included in cosmetics may not be easy because the viscosity is too high.

Ingredients of the composition Moisture retention over time ( % ) 30 minutes to dry 1 hour to dry 2 hours to dry 3 hours to dry 4 hours to dry 5 hours to dry dry 6 hours 15 hours to dry Example One CM-CNF+HA 89.8 77.07 58.44 31.38 19.01 8.76 2.72 0.5 Example 2 CM-CNF+HA 88.25 75.29 52.64 24.35 10.19 0.81 0.51 0.51 Example 3 CM-CNF+HA 87.45 74.45 51.53 21.87 7.79 0.76 0.51 0.5 comparative example One CM-CNF 86.4 74.21 48.11 18.17 2.84 0.5 0.5 0.5 comparative example 2 HA 87.05 77.3 46.58 16.56 3.18 0.51 0.51 0.51 comparative example 3 CMC+HA 89.68 72.9 46.19 10.88 1.75 0.59 0.5 0.5 comparative example 4 CMC 82.42 63.59 35.87 1.21 0.58 0.5 0.5 0.5

Based on the values shown in Table 2, the water retention rate over time was graphically shown in FIGS. 1 to 3.

1 is a graph showing the moisture retention rate over time of the moisturizing compositions according to Examples 1 to 3. The mixing ratio of the carboxymethyl cellulose nanofibers and the hyaluronic acid of Examples 1 to 3 was different, and it was confirmed that the viscosity and water retention rate varied according to the mixing ratio, and the water retention rate over time of Example 1 was the most high was found.

Figure 2 is a graph showing the water retention rate over time in Example 1 and Comparative Examples 1 and 2, Figure 3 is a graph showing the water retention rate over time in Example 1 and Comparative Examples 3 and 4.

According to Table 2, it can be seen that Examples 1 to 3 have higher water retention rates after 2 hours of drying than Comparative Examples 1 to 4. In particular, it can be seen that Examples 1 to 3 and Comparative Examples 1 to 4 have a large difference in moisture retention at 3 to 4 hours of drying.

In addition, comparing the water retention rate measured at 5 hours of drying, Example 1 was 8.76%, but Comparative Examples 1 to 4 were confirmed to be very different at about 0.5%.

Although the preferred embodiments of the present invention have been described above, the present invention is not limited thereto, and various modifications and implementations are possible within the scope of the claims and the detailed description of the invention, and this also belongs to the scope of the invention. .

Claims (8)

It contains carboxymethylated cellulose nanofibers and hyaluronic acid, and has a viscosity of 600 cP to 750 cP at 25 ° C,
The carboxymethylated cellulose nanofibers have a diameter of 10 nm to 60 nm,
The mixing ratio of the carboxymethylated cellulose nanofibers and the hyaluronic acid is 3: 7 to 7: 3 by weight of the moisturizing composition. The moisturizing composition according to claim 1, wherein the moisture retention rate at a drying temperature of 32°C, a relative humidity of 25%, and drying for 4 hours is 7% or more. The method according to claim 1, wherein the carboxymethylated cellulose nanofiber content is 0.1 to 5% by weight relative to 100% by weight of the moisturizing composition, the hyaluronic acid content is 0.1 to 5% by weight relative to 100% by weight of the moisturizing composition Moisturizing composition. delete The method according to claim 1, The content of the carboxymethylated cellulose nanofibers and hyaluronic acid is 0.2 to 1% by weight of the moisturizing composition compared to 100% by weight of the moisturizing composition. A mask pack comprising the moisturizing composition of any one of claims 1 to 3 and 5 as a lotion. A cosmetic comprising the moisturizing composition of any one of claims 1 to 3 and 5. preparing carboxymethylated cellulose by modifying cellulose fibers;
Nanonizing the carboxymethylated cellulose; and
A method for preparing a moisturizing composition according to any one of claims 1 to 3 and 5, comprising the step of preparing a moisturizing composition comprising carboxymethylated cellulose nanofibers and hyaluronic acid.