KR102337054B1 - Hydrogel Composition - Google Patents

Abstract

A hydrogel composition comprising 3 to 10% by weight of an acrylic resin, 5 to 30% by weight of a polyhydric alcohol, 0.1 to 0.5% by weight of a curing agent, 1 to 20% by weight of charcoal powder, and 50 to 80% by weight of purified water is disclosed. The hydrogel composition of the present invention is prepared by adding charcoal powder as a modifier to a hydrogel formed using an acrylic resin as a main material, and not only improves the processability of the hydrogel product, but also has excellent elasticity and softness. great. These hydrogel products can be applied to sheet-type mask packs that deliver cosmetic ingredients.

Description

Hydrogel Composition {Hydrogel Composition}

The present invention relates to a hydrogel composition, and more particularly, by adding charcoal powder as a modifier to a hydrogel formed using an acrylic resin as a main material, not only improves processability, but also has excellent elasticity and softness. It relates to a hydrogel composition.

A hydrogel is a material having a three-dimensional hydrophilic polymer network structure using purified water as a dispersion medium, and has the ability to absorb a large amount of water and also has flexibility. Therefore, hydrogels are often used as a delivery medium for pharmaceuticals or cosmetic agents, and in particular, they are often applied to mask packs that deliver cosmetic ingredients.

Such a hydrogel product can be prepared by mixing an acrylic resin such as polyacrylate as a main material for forming a matrix with a small amount of a curing agent and containing purified water. However, when a hydrogel product is manufactured using only acrylic resin as the main material, it is difficult to manufacture in a sheet shape because the fluidity is too large, and when the hydrogel is attached to the nonwoven substrate, the hydrogel penetrates into the back of the nonwoven substrate, resulting in marketability. There is a problem of this falling, and also there is a problem that the cut surface is not formed neatly when the hydrogel product formed on the nonwoven substrate is cut to an appropriate size.

Due to this problem, attempts have been made to solve the processability problem by further adding a modifier for forming a matrix, such as CMC, kaolin, gelatin, etc. to the acrylic resin.

Specifically, Patent Registration No. 10-0809488 (registered on February 26, 2008) discloses a composition for a sheet-type hydrogel pack and a method for manufacturing a sheet-type hydrogel pack using the same. The disclosed hydrogel composition comprises kaolin, acrylate, Carboxymethylcellulose (CMC), sulfur, titanium, zinc oxide, allantoin, glycerin, sorbitol, gelatin, distilled water, illite and fragrance. These sheet-type hydrogel packs exhibit excellent keratin removal, cosmetic ingredients and moisture supply effects within a short adhesion time, and at the same time, there is almost no residual skin of the pack agent during peeling from the skin. It can be very useful for removal.

According to the research of the present inventors, if the hydrogel is formed by adding a modifier that forms a matrix, such as CMC, kaolin, gelatin, etc. to the acrylic resin, the above processability problem can be solved, but such a hydrogel product adheres to the skin It was found that there was a problem in that it felt uncomfortable and hard to the user, thereby reducing the satisfaction in use.

Accordingly, the present inventors studied a hydrogel product capable of improving processability as well as further improving the feeling of satisfaction in use. As a result, the present invention has been reached.

Accordingly, an object of the present invention is to provide a hydrogel composition that not only improves processability, but also has excellent elasticity and excellent softness.

It is also an object of the present invention to provide a hydrogel composition having improved stability without irritation and toxicity, and has nature-friendly properties.

The hydrogel composition according to the present invention for achieving the above object is 3 to 10% by weight of an acrylic resin, 5 to 30% by weight of a polyhydric alcohol, 0.1 to 0.5% by weight of a curing agent, 1 to 20% by weight of charcoal powder, and 50 to 80% by weight of purified water % by weight.

In the above, the charcoal powder is preferably included in an amount of 1 to 15% by weight, the charcoal powder is more preferably included in an amount of 1 to 10% by weight, and the charcoal powder is more preferably included in an amount of 2 to 10% by weight. desirable.

The acrylic resin may be composed of 3 to 9 wt% of a polyacrylate resin and 0.5 to 2 wt% of a polyacrylic acid resin.

The polyhydric alcohol is preferably glycerin or butylene glycol.

The curing agent is preferably aluminum glycinate (Aluminum Glycinate), aluminum hydroxide or magnesium aluminum silicate (Magnesium Aluminum Silicate).

It is preferable to further include 0.1 to 0.5% by weight of tartaric acid, 0.1 to 0.5% by weight of EDTA-2Na, and 0.1% by weight of a preservative as a pH adjuster.

The acrylic resin may be composed of 4 to 5% by weight of the polyacrylate resin, and the charcoal powder may be composed of 2 to 4% by weight of the polyacrylate resin.

The acrylic resin may be composed of 4.5 to 5% by weight of polyacrylate resin and 0.5 to 2% by weight of polyacrylic acid resin, and the charcoal powder may be composed of 2 to 5% by weight of polyacrylate resin.

The hydrogel composition of the present invention is prepared by adding charcoal powder as a modifier to a hydrogel formed using an acrylic resin as a main material, and not only improves the processability of the hydrogel product, but also has excellent elasticity and softness. great. These hydrogel products can be applied to sheet-type mask packs that deliver cosmetic ingredients.

1 is a view showing a curved surface adhesion test apparatus for measuring the curved surface adhesion properties for a hydrogel product manufactured according to an embodiment of the present invention.

Hereinafter, the present invention will be described in detail.

The hydrogel composition of the present invention comprises 3 to 10% by weight of an acrylic resin, 5 to 30% by weight of a polyhydric alcohol, 0.1 to 0.5% by weight of a curing agent, 1 to 20% by weight of charcoal powder, and 50 to 80% by weight of purified water. In addition to the above components, the hydrogel composition of the present invention may further include 0.1 to 0.5% by weight of tartaric acid, 0.1 to 0.5% by weight of EDTA-2Na, and 0.1% by weight of a preservative as a pH adjuster. Here, tartaric acid acts as a pH adjuster, and EthyleneDiamineTetraAcetic acid (EDTA) acts as a reaction rate adjuster. In addition, a cosmetic ingredient for skin care or a drug for treating skin-related diseases may be further included.

The components constituting the matrix in the hydrogel composition of the present invention include an acrylic resin, a curing agent and charcoal powder. Here, the component constituting the matrix means a component forming the solid content of the hydrogel.

In the hydrogel composition of the present invention, the acrylic resin is included in an amount of 3 to 10% by weight, preferably 4 to 9% by weight. The present invention can be used without particular limitation as long as it is an acrylic resin used to prepare a sheet-type hydrogel product containing a drug or cosmetic ingredient. When the content of the acrylic resin is too small, it is not preferable because the hydrogel property to absorb water is insufficient. there will be no

In the hydrogel composition of the present invention, the acrylic resin may be composed only of a polyacrylate resin, but may be composed of 3 to 9% by weight of polyacrylate resin, preferably 4 to 7% by weight, and 0.5 to 2% by weight of polyacrylic acid resin have.

Charcoal powder used in the hydrogel composition of the present invention is used to have a particle size of about 200 to 400 mesh, in addition to the charcoal powder, graphite powder and carbon powder may be used. Charcoal powder in the composition of the present invention is a shape-retaining modifier for the hydrogel, which improves processability for the hydrogel, that is, the surface adhesion to the non-woven fabric, so that the hydrogel composition does not penetrate into the inner surface of the non-woven fabric, thereby producing a hydrogel product. It has the characteristics of making it easy and improving the cutting property. In addition, the charcoal powder also serves to facilitate the preparation of the hydrogel composition of the present invention in a desired shape.

Charcoal powder is also a nature-friendly material itself, so it has less irritation and toxicity, and also has the advantage of excellent safety because it does not cause pathogenicity or safety problems due to material denaturation compared to animal-derived materials such as gelatin. Charcoal powder in the hydrogel composition of the present invention also allows the hydrogel product to have excellent softness while having excellent elasticity. Moreover, charcoal powder also has the advantage of being inexpensive compared to modifiers used in the prior art, for example, CMC, kaolin, gelatin, and the like. The hydrogel composition of the present invention also has a secondary property of improving the adsorption property to wastes of the skin by charcoal.

Charcoal powder in the hydrogel composition of the present invention may be used in 1 to 20% by weight, preferably 1 to 15% by weight, more preferably 1 to 10% by weight, more preferably may be used in an amount of 2 to 10% by weight, 3 to 10% by weight, or 5 to 10% by weight.

Specifically, when the acrylic resin in the hydrogel composition of the present invention consists of 4 to 5% by weight of the polyacrylate resin, the charcoal powder is preferably added in an amount of 2 to 4% by weight. In particular, when the acrylic resin is composed of 5% by weight of the polyacrylate resin, the charcoal powder is preferably added in an amount of 3% by weight. In addition, when the acrylic resin is composed of 4.5 to 5% by weight of the polyacrylate resin and 0.5 to 2% by weight of the polyacrylic acid resin, the charcoal powder is preferably composed of 2 to 5% by weight, particularly 3% by weight.

In the hydrogel composition of the present invention, the curing agent generally used to form a hydrogel may be employed, and in particular, aluminum glycinate (Aluminum Glycinate), aluminum hydroxide or magnesium aluminum silicate may be used.

In the hydrogel composition of the present invention, the polyhydric alcohol is preferably glycerin or butylene glycol. In addition, polyhydric alcohols such as propylene glycol and diethylene glycol may be used. In the hydrogel composition of the present invention, glycerin, etc. serves as a dispersant for the matrix component, and is mixed with purified water so that the cosmetic component contained in the hydrogel is well dispersed in the purified water. It also serves as a shape-forming agent. Glycerin is also mixed with purified water contained in the hydrogel to keep the hydrogel in a wet state, and also serves as a moisturizer by providing adequate volatilization to moisture.

Glycerin is preferably included in 5 to 30% by weight in the hydrogel composition of the present invention, more preferably 15 to 25% by weight, and specifically included in about 20% by weight. When glycerin is included in too small an amount, it becomes insufficient to exhibit the above-mentioned functions, and when included in too large amount, the content of other components and purified water decreases, so that it is impossible to balance the required properties as a whole.

In the hydrogel composition of the present invention, purified water is contained in an amount of 50 to 80% by weight. If the content of purified water in the hydrogel composition of the present invention is too small, it is not possible to sufficiently exhibit the properties of the hydrogel. On the other hand, the maximum content of purified water is dependent on the properties of the matrix formed by the acrylic resin, curing agent and charcoal powder, the maximum content of purified water in the hydrogel composition of the present invention is about 80% by weight.

Hereinafter, the present invention will be described in more detail by way of Examples. However, since the examples described below are merely illustrative of the present invention, it should not be understood that the scope of the present invention is limited thereby.

Example

< Example 1-11>

A hydrogel composition composed of components and component ratios as shown in the table below was prepared. A sheet was formed with the hydrogel composition thus prepared and tested for curved adhesion, elongation, elastic recovery, back penetration, cutting, loss on drying and drug release.

The curved adhesion test was performed by attaching a specimen of a 30 x 60 mm rectangular hydrogel sheet (1000 g/m ² ) to the upper part of a 52 mm diameter hemispherical device made of transparent plastic (PET), as shown in FIG. 1, for 1 hour. After that, the attachment state was observed.

For the elongation test, a hydrogel sheet having a thickness of 20 x 70 mm and a thickness of 2 mm was used as a specimen. UTM was used as the device used. The length of the specimen to be tested was 50 mm by attaching 10 mm each of both ends of the specimen to a tensile testing machine (UTM). The length of breakage was measured by stretching the specimen to one side.

Elongation = (L - L ₀ )/L ₀ x 100 (%)

* L: extended length, L ₀ : initial specimen length

For the elastic recovery rate test, a hydrogel sheet having a thickness of 10 x 50 mm and 5 mm was used as a specimen. After stretching the specimen to three times (150mm) of its length in the horizontal direction, the restored length was checked to determine the horizontal elastic recovery factor, and the restored length after stretching the specimen to three times (150mm) of its length in the vertical direction It was determined as the vertical elastic recovery factor. However, when measuring in the vertical direction, the length extended by gravity was excluded.

Elastic recovery factor = [1 - (L ₁ - L ₀ )/L] x 100 (%)

* L: Extended length (100mm), L ₁ : Extended length, L ₀ : Initial specimen length

For the cutting property test, a ^{hydrogel sheet having a weight of 1000 g/m 2} attached to the nonwoven fabric was used as a specimen. The internal mechanism (die roll) was used as a device to be used. The cutting property of the gel was confirmed when the sheet was half-cut.

Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 polyacrylate resin
6.50
6.50
6.50
6.50
5.00
5.00
5.00 polyacrylic acid resin glycerin 20.00 20.00 20.00 25.00 20.00 20.00 23.00 aluminum glycinate 0.14 0.14 0.14 0.14 0.14 0.14 0.14 TTA 0.27 0.27 0.27 0.27 0.27 0.27 0.27 EDTA-2Na 0.14 0.14 0.14 0.14 0.14 0.14 0.14 antiseptic 0.10 0.10 0.10 0.10 0.10 0.10 0.10 CMC kaolin gelatin Charcoal 1.00 3.00 5.00 10.00 3.00 5.00 10.00 water 71.85 69.85 67.85 57.85 71.35 69.35 61.35

* TTA: Tartaric acid

* CMC: Carboxymethylcellulose

Example 6 Example 8 Example 9 Example 10 Example 11 polyacrylate resin 5.00 5.00 4.50 4.00 3.50 polyacrylic acid resin 0.70 0.70 0.70 00.7 glycerin 20.00 20.00 20.00 20.00 20.00 aluminum glycinate 0.14 0.14 0.14 0.14 0.14 TTA 0.27 0.27 0.27 0.27 0.27 EDTA-2Na 0.14 0.14 0.14 0.14 0.14 antiseptic 0.10 0.10 0.10 0.10 0.10 CMC kaolin gelatin Charcoal 5.00 5.00 5.00 5.00 5.00 water 69.35 68.65 69.15 69.65 70.15

< comparative example 1-6>

For comparison with the above Examples, a hydrogel composition of Comparative Example was prepared with the components and component ratios as shown in the table below. The hydrogel composition thus prepared was used to form a sheet and tested for curved adhesion, elongation, elastic recovery, back penetration, cutting, loss on drying and drug release.

Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Comparative Example 6 polyacrylate resin 6.50 6.50 6.50 5.00 5.00 5.00 polyacrylic acid resin glycerin 20.00 20.00 20.00 20.00 20.00 20.00 aluminum glycinate 0.14 0.14 0.14 0.14 0.14 0.14 TTA 0.27 0.27 0.27 0.27 0.27 0.27 EDTA-2Na 0.14 0.14 0.14 0.14 0.14 0.14 antiseptic 0.10 0.10 0.10 0.10 0.10 0.10 CMC 2.00 2.00 2.00 2.00 kaolin 3.00 3.00 3.00 3.00 gelatin 3.00 3.00 Charcoal water 72.85 67.85 64.85 74.35 69.35 66.35

<Test result>

Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Adhesion to curved surfaces (1hr,min) clear elongation (mm) 791 508 458 276 429 408 256 (%) 1482% 916% 816% 452% 758% 716% 412% elastic recovery rate vertical 95% 98.50% 100% 100% 97% 100% 100% horizontal 90% 100% 100% 100% 92% 100% 100% dorsal penetration non-penetrating Cutability (Side Cut) NG OK Loss on drying (after 4 hours, %) 75.67 76.23 78.16 81.15 73.26 76.92 80.94 Drug release (min) 60 24hr↑ 24hr↑ 24hr↑ 60 24hr↑ 24hr↑

Example 6 Example 8 Example 9 Example 10 Example 11
Adhesion to curved surfaces (1hr,min) clear 50 45 clear elongation (mm) 408 266 270 337 273 (%) 716% 432% 440% 574% 446% elastic recovery rate vertical 100% 100% 100% 100% 100% horizontal 100% 100% 100% 100% 100% dorsal penetration non-penetrating Cutability (Side Cut) OK NG NG Loss on drying (after 4 hours, %) 76.92 79.46 77.35 72.85 70.77 Drug release (min) 24hr↑ 55 55 50 50

Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Comparative Example 6
Adhesion to curved surfaces (1hr,min) clear elongation (mm) 550 342 498 not measurable 356 404 (%) 1000% 584% 896% not measurable 612% 708% elastic recovery rate vertical 90% 98% 100% not restored 98% 100% horizontal 87% 90% 90% not restored 90% 88% dorsal penetration Penetration non-penetrating Penetration non-penetrating Cutability (Side Cut) NG OK NG OK Loss on drying (after 4 hours, %) 79.82 81.68 79.58 71.40 79.74 77.07 Drug release (min) 60 90 120 50 55 65

<review>

First, as a comparative example, the hydrogel sheet products prepared according to Comparative Examples 1 and 4 containing only an acrylic resin and a curing agent as matrix components are molded in which the hydrogel penetrates into the back surface of the nonwoven substrate when the hydrogel sheet is attached on the nonwoven substrate. There was a gender problem. In addition, the cutting ability was not good, so the processability was not good.

In addition, the product of Comparative Example 1 generally had poor elastic recovery. In particular, the hydrogel sheet product of Comparative Example 4, in which the content of the acrylic resin was relatively small, could not measure the elongation, and was not restored at all when it was stretched only by a predetermined length to measure the elastic recovery rate and then placed.

The hydrogel sheet products of Comparative Examples 2, 3, 5 and 6, in which CMC, kaolin, and gelatin were further added in addition to the acrylic resin and curing agent as matrix components, when the hydrogel sheet was attached on the nonwoven substrate, the hydrogel sheet was applied to the back surface of the nonwoven substrate. There was no problem in moldability through which the gel penetrated, and there was no problem in cutting property, so the processability was good. However, the formability and processability were improved to a satisfactory level by the addition of CMC, kaolin and gelatin, but compared with the hydrogel sheet products according to the embodiments of the present invention, the hydrogel sheet products of Comparative Examples were CMC, kaolin and gelatin. Compared to the added amount, the elastic recovery rate was not significantly improved. In particular, when considering both elongation and elastic recovery, it was confirmed that the hydrogel sheet products of Comparative Examples had inferior elastic properties compared to the hydrogel sheet products of Examples of the present invention.

The hydrogel sheet products prepared according to the embodiments of the present invention generally satisfied the properties of curved adhesion, elongation, elastic recovery, back penetration, cutting and drug release.

Specifically, looking at the properties of the hydrogel sheet product of Example 1, it can be confirmed that the elastic recovery rate was significantly improved compared to the product of Comparative Example 1, even though only a small amount of charcoal powder was added at 1 wt%. This confirms that the elastic recovery rate is improved to a level corresponding to the addition of a small amount of charcoal powder compared to the product of Comparative Example 2, in which the addition amount of CMC and kaolin is 5% by weight, so that the charcoal powder is compared to the modifier according to the prior art. It shows excellent performance. In particular, the product of Example 1 has a higher elastic recovery rate than the product of Comparative Example 1 despite the elongation rate being greater than that of Comparative Example 1, which supports that the product of Example 1 has both elasticity and softness properties. .

The product of Example 1 shows rather poor characteristics in cutability, which has room for improvement by establishing other process conditions. The problem is estimated to be solvable.

Compared to the product of Example 1, the product of Example 2 obtained even good cutting properties as the amount of charcoal powder increased to 3 wt%. That is, it has uniformly satisfactory characteristics in curved adhesion, elongation, elastic recovery, back penetration, and cutting properties. However, in drug-releasing properties, the time it takes for the drug contained in the hydrogel at the boundary of the nonwoven substrate to be absorbed into the skin in the hydrogel sheet product exceeds 24 hours. This drug-releasing property is disadvantageous because the hydrogel sheet product must contain more cosmetic ingredients than necessary, but it does not act as a disqualification for use.

Compared to the products of Examples 1 and 2, the product of Example 3 had an elastic recovery rate characteristic increased to a perfect level as the amount of charcoal powder was increased to 5% by weight. However, in the drug-releasing properties, as in the product of Example 2, the time it takes for the drug contained in the hydrogel at the boundary of the non-woven substrate to be absorbed into the skin in the hydrogel sheet product exceeds 24 hours.

As the amount of charcoal powder added increases, as shown in Example 4, the elasticity is further improved, and the elongation is decreased. However, even at this time, the elongation is sufficient to be used as a hydrogel sheet product. It is considered that the increase in elasticity and the decrease in elongation according to the addition of charcoal powder show that the softness is conversely decreased while the elasticity is increased. However, the softness characteristic does not necessarily correspond to the elongation, and it is considered that it shows a tendency characteristic only with respect to the addition of the same material. Therefore, the hydrogel sheet product within the scope of the present invention exhibits good product properties by simultaneously satisfying elastic properties and softness properties.

On the other hand, in the product of Example 5, the content of acrylic resin (polyacrylate resin) was reduced to 5% by weight and the amount of charcoal powder added was selected to be 3% by weight. shows

The products of Examples 6 and 7 show that when the amount of charcoal powder is increased to 5% by weight and 10% by weight in a state where the content of the acrylic resin (polyacrylate resin) is reduced to 5% by weight, the drug release property is deteriorated again. .

However, Example 8 shows that when the content of the acrylic resin is 5% by weight of the polyacrylate resin and 0.7% by weight of the polyacrylic acid resin is added, and the amount of charcoal powder is 5% by weight, the drug release property is improved again. This shows that if the acrylic resin in the present invention is selected in an appropriate ratio between the acrylate resin and the acrylic acid resin, all the physical properties required for the hydrogel sheet product can be almost perfectly prepared.

On the other hand, in the product of Example 8, the hydrogel sheet attached to the curved surface in 50 minutes in the curved surface adhesion test fell off the curved surface, which can be said to have somewhat poor properties compared to other Examples and Comparative Examples in curved surface adhesion. However, since a cosmetic pack made of a hydrogel sheet is usually used by attaching it to the face for about 30 minutes, it can be said that the degree of adhesiveness to the curved surface satisfies the physical properties required for the hydrogel sheet cosmetic pack.

Next, the product of Example 9 is to reduce the content of the polyacrylate resin to 4.5% by weight in the component ratio of the product of Example 8, and satisfactorily equipped with all the physical properties required for the hydrogel sheet product. However, the adhesive properties of the curved surface are only about 45 minutes, but, as mentioned above, that is enough to satisfy the physical properties required for the hydrogel sheet cosmetic pack.

Next, the product of Example 10 was obtained by reducing the content of the polyacrylate resin to 4% by weight in the component ratio of the product of Example 9. In this case, it was confirmed that the adhesiveness to the curved surface was improved while the cutability was poor. This trend was also confirmed in the product of Example 11, in which the content of the polyacrylate resin was reduced to 3.5 wt%.

From the above results, the hydrogel sheet product of the present invention has almost the physical properties of the hydrogel sheet used as a cosmetic pack by appropriately adjusting the component ratio of the acrylic resin, particularly the composition ratio of polyacrylate resin and polyacrylic acid resin, and the component ratio of charcoal powder. It was confirmed that it could be completely satisfied.

Claims (10)

In the hydrogel composition,
The hydrogel composition comprises 4 to 9% by weight of an acrylic resin, 5 to 30% by weight of a polyhydric alcohol, 0.1 to 0.5% by weight of a curing agent, 2 to 10% by weight of charcoal powder, and 50 to 80% by weight of purified water,
The matrix of the hydrogel composition is a hydrogel composition, characterized in that consisting only of the acrylic resin, the curing agent and the charcoal powder. delete delete delete delete According to claim 1,
The polyhydric alcohol is a hydrogel composition, characterized in that glycerin or butylene glycol. According to claim 1,
The curing agent is aluminum glycinate (Aluminum Glycinate), aluminum hydroxide or magnesium aluminum silicate hydrogel composition, characterized in that. According to claim 1,
A hydrogel composition comprising 0.1 to 0.5% by weight of tartaric acid, 0.1 to 0.5% by weight of EDTA-2Na, and 0.1% by weight of a preservative as a pH adjusting agent. According to claim 1,
The acrylic resin is composed of 4 to 5% by weight of the polyacrylate resin, and the charcoal powder is a hydrogel composition, characterized in that consisting of 2 to 4% by weight. According to claim 1,
The acrylic resin is composed of 4.5 to 5% by weight of a polyacrylate resin and 0.5 to 2% by weight of a polyacrylic acid resin, and the charcoal powder is a hydrogel composition, characterized in that consisting of 2 to 5% by weight.

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