KR20200130572A - Mask pack sheet product using low substituted carboxymethyl cellulose nonwoven fabrics and method for producing using the same - Google Patents

Abstract

Disclosed are: a mask pack sheet product using a low-substituted carboxymethyl cellulose non-woven fabric, in which a substitution degree of a carboxymethyl group of a cellulose non-woven fabric is adjusted by 0.05 to 0.3, such that moisture retention and transparent properties are increased; and a manufacturing method of the mask pack sheet product. According to the present invention, the manufacturing method comprises the following steps: (a) immersing a cellulose non-woven fabric in an alkali solution to perform pretreatment; (b) squeezing the pretreated cellulose non-woven fabric; (c) dissolving a carboxymethylation agent in water to prepare a reception solution; (d) adding the squeezed cellulose non-woven fabric to the reception solution to substitute a hydroxy group placed at an end of the cellulose non-woven fabric with a carboxymethyl group, wherein the substitution degree of the carboxymethyl group is 0.05 to 0.3; and (e) pressing and drying the substituted cellulose non-woven fabric.

Description

A mask pack sheet product using a low-substituted carboxymethyl cellulose nonwoven fabric and its manufacturing method {MASK PACK SHEET PRODUCT USING LOW SUBSTITUTED CARBOXYMETHYL CELLULOSE NONWOVEN FABRICS AND METHOD FOR PRODUCING USING THE SAME}

The present invention relates to a mask pack sheet product using a low-substituted carboxymethyl cellulose nonwoven fabric, and to a mask pack sheet product in which water retention and transparency are improved by adjusting the degree of substitution of the carboxymethyl group of the cellulose nonwoven fabric to 0.05 to 0.3, and a manufacturing method thereof. .

The mask pack sheet is attached to the skin surface and removed after a certain period of time, and is used to supply the moisture, oil and nutrition contained in the mask pack sheet to the skin.

Existing mask pack sheets are manufactured by using cellulose fiber materials and materials such as polypropylene and polyethylene terephthalate alone, or by mixing them.

Among these, mask pack sheets made of synthetic materials such as polypropylene and polyethylene terephthalate have low adhesion and water retention properties to the skin, so they have a disadvantage of low ability to deliver functional active ingredients such as moisturizing, soothing, and elasticity to the skin. .

On the other hand, cellulose fiber is an eco-friendly polymer, and a large number of cellulose unit molecules are gathered to form a fiber. Cellulose fibers are composed of a crystalline region and an amorphous region, and when immersed in water, a liquid permeates the amorphous region and swells. Due to these properties, it is known that a mask pack sheet using cellulose fibers is excellent in adhesion and water retention to the skin.

However, as materials having expensive water retention and transparency such as hydrogels are developed, cellulose fibers have limitations in exhibiting the level of water retention and transparency required by consumers. Nevertheless, there is a constant demand for cellulose fibers that are natural materials and are excellent in price/performance.

Therefore, there is a need for a mask pack sheet that satisfies water retention and transparency at the same time and has excellent performance for the price.

KR 10-2015-0050808 (published on May 11, 2015)

An object of the present invention is to provide a mask pack sheet product excellent in water retention and transparency.

In addition, an object of the present invention is to provide a method of manufacturing a mask pack sheet product in which the concentration of a carboxymethylating agent is controlled in order to adjust the degree of substitution of the carboxymethyl group to 0.05 to 0.3.

The objects of the present invention are not limited to the above-mentioned objects, and other objects and advantages of the present invention that are not mentioned can be understood by the following description, and will be more clearly understood by examples of the present invention. In addition, it will be easily understood that the objects and advantages of the present invention can be realized by the means shown in the claims and combinations thereof.

The mask pack sheet product according to the present invention includes a cellulose nonwoven fabric having a terminal substituted with a carboxymethyl group, and the cellulose nonwoven fabric has a carboxymethyl group substitution degree of 0.05 to 0.3.

A method of manufacturing a mask pack sheet product according to the present invention comprises the steps of: (a) pretreating a cellulose nonwoven fabric by immersing it in an alkali solution; (b) squeezing the pretreated cellulose nonwoven fabric; (c) preparing a reaction solution by dissolving a carboxymethylating agent in water; (d) adding the squeezed cellulose nonwoven fabric to the reaction solution, and substituting a hydroxy group at the end of the cellulose nonwoven fabric with a carboxymethyl group; And (e) drying the substituted cellulose nonwoven fabric after nonwoven fabrication; and, in the step (d), the substitution is performed to have a carboxymethyl group substitution degree of 0.05 to 0.3.

The mask pack sheet product according to the present invention is obtained by substituting a hydroxy group at the end with a carboxymethyl group, and having a degree of substitution of a carboxymethyl group of 0.05 to 0.3, has an effect of showing excellent water retention and transparency (when absorbed).

In addition, according to the present invention, by dissolving the carboxymethylating agent in water and adjusting the concentration of the reaction solution, a low-substituted mask pack sheet product can be manufactured.

In addition to the above-described effects, specific effects of the present invention will be described together while describing specific details for carrying out the present invention.

1 is a flow chart showing a method of manufacturing a mask pack sheet product using a low-substituted carboxymethyl cellulose nonwoven fabric according to the present invention.
2 is a photograph of a CMC nonwoven fabric manufactured according to Example 4 of the present invention.
3 is a photograph of a CMC nonwoven fabric manufactured according to Comparative Example 1 of the present invention.

The above-described objects, features, and advantages will be described later in detail with reference to the accompanying drawings, and accordingly, one of ordinary skill in the art to which the present invention pertains will be able to easily implement the technical idea of the present invention. In describing the present invention, if it is determined that a detailed description of known technologies related to the present invention may unnecessarily obscure the subject matter of the present invention, a detailed description will be omitted. Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. In the drawings, the same reference numerals are used to indicate the same or similar elements.

In addition, when a component is described as being "connected", "coupled" or "connected" to another component, the components may be directly connected or connected to each other, but other components are "interposed" between each component. It is to be understood that "or, each component may be "connected", "coupled" or "connected" through other components.

Hereinafter, a mask pack sheet product using a low-substituted carboxymethyl cellulose nonwoven fabric according to an embodiment of the present invention and a method of manufacturing the same will be described.

In the present invention, a reaction solution obtained by dissolving a carboxymethylating agent in water, and a concentration of the reaction solution are controlled to prepare a mask pack sheet product having a carboxymethyl group substitution degree of 0.05 to 0.3 of a cellulose nonwoven fabric. The low-substituted carboxymethyl cellulose of the present invention refers to cellulose having a degree of substitution of a carboxymethyl group from 0.05 to 0.3.

1 is a flow chart showing a method of manufacturing a mask pack sheet product using a low-substituted carboxymethyl cellulose nonwoven fabric according to the present invention.

Referring to FIG. 1, the method of manufacturing a mask pack sheet product of the present invention includes pretreatment by immersing a cellulose nonwoven fabric in an alkali solution (S110), squeezing (S120), and dissolving a carboxymethylating agent in water. A step of preparing (S130), a step of replacing by adding the squeezed cellulose nonwoven fabric to the reaction solution (S140), and a step of drying after pressing (S150).

Pre-treatment by immersing the cellulose nonwoven fabric in an alkali solution (S110)

This step is a process of immersing and aging the cellulose nonwoven fabric in an alkaline solution to facilitate the reaction process. If the pretreatment process is not sufficiently performed, the pretreatment process is very important because a substitution reaction or the like does not occur. Since the fabric properties change depending on the temperature and time of the pretreatment process, the pretreatment process is a process that requires careful control.

The cellulose nonwoven fabric used in the present invention refers to natural cellulose fibers having a repeating unit of 200 to 5000. If the repeating unit is less than 200, it may be difficult to maintain the sheet shape due to the decrease in the strength of the fiber. Conversely, if the repeating unit exceeds 5000, dissociation of the hydroxyl group by alkali weakens and it may be difficult to control the degree of substitution.

The alkali solution in which the cellulose nonwoven fabric is immersed has a concentration of 15 to 40%. Alkaline solution is used by mixing one or more chemical substances with high alkali such as sodium hydroxide (NaOH), potassium hydroxide (KOH), aqueous ammonia (NH ₄ OH), or trimethyl ammonium hydroxide. It is possible. Among these, it is preferable to use sodium hydroxide as the alkaline solution.

When the concentration of the alkali solution is less than 15%, it is difficult to obtain the required degree of substitution due to low alkalinity. On the contrary, if it exceeds 40%, the degree of substitution with the carboxymethyl solution increases and the degree of substitution is excessively high, or side reactions may occur, resulting in deterioration of the physical properties of the fabric.

After immersing the cellulose nonwoven fabric in an alkaline solution, it must undergo a aging process. Maturation is a process for dissociating hydrogen bonds of cellulose molecules, and usually proceeds at a temperature of 20 to 70°C. If the temperature is lower than 20℃, it takes too much time for proper aging. If the temperature exceeds 70℃, overreaction may occur, resulting in embrittlement of fibers. Also, the maturation time must be adjusted. Since the aging time varies depending on the mixing ratio, immersion time, aging temperature, and characteristics of equipment, it is desirable to optimize the final nonwoven fabric by measuring the degree of substitution.

Squeezing step (S120)

Subsequently, the aged cellulose nonwoven fabric must be properly squeezed while passing through two rolls with which pressure is controlled.

Squeeze is a very important factor in determining the amount of alkali solution remaining in the nonwoven fabric, leaving only a desired part of the alkali solution used for aging in the nonwoven fabric and removing the remaining amount. Squeeging determines the fabric pickup rate by controlling the pressure between the rolls, and the pickup rate is preferably 200 to 500%. The pickup rate (%) represents the amount of the alkali solution remaining in the cellulose nonwoven fabric after immersion as a ratio of the dry weight of the cellulose nonwoven fabric. That is, the pickup rate (%) is {(wet weight-dry weight)/dry weight}×100.

If the pickup rate is less than 200%, the dissociation of hydrogen bonds of the cellulose molecule may be insufficient, making it difficult to control the degree of substitution. Conversely, if the pickup rate exceeds 500%, the dissociation of hydrogen bonds of the cellulose molecule may be excessive, and the degree of substitution may be excessively high.

Therefore, it is important to appropriately control the squeezing so that the pick-up rate of the cellulose nonwoven fabric with respect to the alkali solution is 200 to 500%.

Dissolving a carboxymethylating agent in water to prepare a reaction solution (S130)

After aging, a reaction solution is prepared by dissolving a carboxymethylating agent in water.

The carboxymethylating agent is a drug in which carboxymethyl can be substituted on the cellulose nonwoven fabric, and halogenated acetic acid such as monochloroacetic acid, monobromoacetic acid, and monoiodoacetic acid, or a neutralized product thereof may be used.

The carboxymethylating agent is the most important factor in determining the degree of substitution, and it is preferable to prepare a reaction solution by dissolving 20 to 60% by weight of the carboxymethylating agent in 40 to 80% by weight of water. When the addition amount of the reaction solution is less than 20% by weight, there is a problem that the degree of substitution is lowered, and when it exceeds 60% by weight, over-substitution may occur.

In addition, to prevent side reactions, distilled water, ion-exchanged water, or RO water (water filtered by reverse osmosis) from which metal components that cause side reactions have been removed may be used as the water used. When the metal content in the water exceeds 50 ppm, side reactions may occur. Here, the metal may be calcium, magnesium, iron, copper, or the like.

Substituting by adding the squeezed cellulose nonwoven fabric to the reaction solution (S140)

Into the prepared reaction solution, a squeezed cellulose nonwoven fabric is added, re-immersed, and heat treated to proceed with a substitution reaction.

At this time, it is preferable to mix so that the weight ratio of the squeezed cellulose nonwoven fabric: reaction solution is 1: 2 to 1: 8, and more preferably to mix so that 1: 4 to 1: 6. When the content of the reaction solution to the squeegeeed cellulose nonwoven fabric is less than 2 times, the content of the reaction solution is insufficient and the substitution reaction rate is low. Conversely, when the content of the reaction solution exceeds 8 times, a problem occurs in that the side reaction rate is increased.

The substitution reaction may induce a reaction through heat treatment at 70 to 150°C, and if it is lower than 70°C, the degree of substitution is low, and if it is higher than 150°C, the fabric may become brittle and the fabric may be torn. In addition, the substitution reaction may proceed within 5 minutes, and if it exceeds 5 minutes, overreaction may occur.

The substitution reaction is to replace a hydroxy group (-OH) located at the end of the dehydrated cellulose nonwoven fabric with an anionic group such as a carboxymethyl group. The carboxymethyl group may be illustrated as -CH ₂ COO ^- Na ⁺ .

The substituted cellulose nonwoven fabric exhibits anionic water solubility, high water retention (protecting/retaining moisture) and high transparency.

After completion of the substitution reaction, water may be washed 2-3 times using water or a mixture of water and an alcohol-based organic solvent to remove unreacted substances from the cellulose nonwoven fabric derivative. At this time, in order to adjust the pH of the substituted cellulose nonwoven fabric, it is preferable to neutralize the pH of the final fabric by adding an acidic chemical such as sulfuric acid, phosphoric acid, hydrochloric acid or formic acid and acetic acid.

Step of drying after compression (S150)

Then, the substituted cellulose nonwoven fabric is compressed and dried to prepare a mask pack sheet product. It is preferable that the manufactured mask pack sheet product is in the form of a nonwoven fabric.

Specifically, after the water washing is finished, it is compressed and dried at 100 to 150°C. If the drying temperature is less than 100°C, sufficient drying of the mask pack sheet product may not be achieved. Conversely, if the drying temperature exceeds 150°C, yellowing may occur in the mask pack sheet product as the temperature increases. In addition, the compression may be performed at 25±10°C, and preferably may be performed by applying pressure at 25±5°C.

The dried mask pack sheet product is immersed in a solution containing at least one skin improvement function among moisturizing, soothing, elasticity, wrinkle improvement, and whitening, so that any one or more of moisturizing, soothing, elasticity, wrinkle improvement and whitening functions It can have an effect.

As described above, in the present invention, a reaction solution in which a carboxymethylating agent is dissolved in water is used, and as the concentration of the reaction solution is adjusted, a mask pack sheet product comprising a low-substituted carboxymethyl cellulose nonwoven fabric having a carboxymethyl group substitution degree of 0.05 to 0.3 Can be manufactured. The mask pack sheet product using the low-substituted carboxymethyl cellulose nonwoven fabric of the present invention exhibits high water retention and transparency, and can be used as a product with excellent performance for the price.

The mask pack sheet product manufactured according to the manufacturing method of the present invention includes a cellulose nonwoven fabric whose end is substituted with a carboxymethyl group. The carboxymethyl group substitution degree of the cellulose nonwoven fabric is characterized in that 0.05 to 0.3.

As the mask pack sheet product is immersed in an essence or solution having a skin improvement function, it may include a component exhibiting at least one skin improvement function among moisturizing, soothing, elasticity, wrinkle improvement, and whitening.

Therefore, the mask pack sheet product of the present invention can be brought into contact with the skin for cosmetic purposes, and provides a skin improvement effect.

As described above, specific examples of the mask pack sheet product using the low-substituted carboxymethyl cellulose nonwoven fabric and a method of manufacturing the same are as follows.

1. Manufacturing of mask pack sheet products

Example 1

For pretreatment, after immersing a cellulose nonwoven fabric satisfying 200 to 5000 repeating units in 20% NaOH aqueous solution, for 15 seconds to dissociate hydrogen bonds of cellulose molecules. It was aged at 25°C. The aged cellulose nonwoven fabric was padded to show a pickup rate of 250%, which was dehydrated and squeegeeed.

Thereafter, a reaction solution in which 30% by weight of monochloroacetic acid (MCA) was dissolved in 70% by weight of distilled water was prepared in the reactor. The squeezed cellulose nonwoven fabric: mixed so that the weight ratio of the reaction solution was 1:5, and the substitution reaction was performed at 90°C for 5 minutes.

Thereafter, a water washing solution obtained by mixing alcohol and distilled water was added to wash twice, and for pH adjustment, a washing solution containing phosphoric acid was added and washed twice. After the completion of washing with water, it was squeezed at 25° C. using an automatic mangle and dried at 140° C. to prepare a carboxymethylcellulose (CMC) nonwoven fabric.

Example 2

A CMC nonwoven fabric was prepared under the same conditions as in Example 1, except that 30% NaOH aqueous solution was used, and the aging for 20 seconds and the pickup rate was 300%.

Example 3

A 40% NaOH aqueous solution was used, and a CMC nonwoven fabric was prepared under the same conditions as in Example 1, except that it was aged for 20 seconds and the pickup rate was 400%.

Example 4

A CMC nonwoven fabric was prepared under the same conditions as in Example 1, except that 40% by weight of monochloroacetic acid (MCA) was dissolved in 60% by weight of distilled water.

Example 5

A CMC nonwoven fabric was prepared under the same conditions as in Example 1, except that it was mixed so that the weight ratio of the squeezed cellulose nonwoven fabric: the reaction solution was 1:4.

Comparative Example 1

A 10% NaOH aqueous solution was used, and a CMC nonwoven fabric was prepared under the same conditions as in Example 1, except that it was aged for 20 seconds and the pickup rate was 190%.

Comparative Example 2

A CMC nonwoven fabric was prepared under the same conditions as in Example 1, except that 10% by weight of monochloroacetic acid (MCA) was dissolved in 90% by weight of distilled water.

Comparative Example 3

A CMC nonwoven fabric was prepared under the same conditions as in Example 1, except that it was mixed so that the weight ratio of the squeezed cellulose nonwoven fabric: the reaction solution was 1:1.

Comparative Example 4

Squeezed cellulose nonwoven fabric: CMC nonwoven fabric was prepared under the same conditions as in Example 1, except that the mixture was mixed so that the weight ratio of the reaction solution was 1:9, and treated at 90°C for 10 minutes.

Comparative Example 5

Squeezed cellulose nonwoven fabric: CMC nonwoven fabric was prepared under the same conditions as in Example 1, except that the mixture was mixed so that the weight ratio of the reaction solution was 1:5, and treated at 60°C for 30 minutes.

2. Physical property evaluation method and results

1) For the mask pack sheet products manufactured in the Examples and Comparative Examples, the degree of substitution was measured according to ASTM D 1439-03. The substitution degree measurement according to the ASTM D 1439-03 method was calculated by applying the following formula, and the results are shown in Table 1.

[Table 1]

2) Water retention: CMC non-woven fabrics prepared in Examples and Comparative Examples were used in the same amount of essence (squalane, xylitol, macadamia seed oil, allantoin, trehalose, tocopherol, glycine, fig extract, centella asiatica extract, jasmine extract, asayaja extract After immersion in 25% by weight of the mixture and 75% of distilled water), the water retention amount over time at 25°C was measured using a moisture measuring device (Corneometer CM825). Table 2 shows the moisture content (%) after 30 minutes.

[Table 2]

3) Transparency upon absorption: After sufficiently absorbing the CMC nonwoven fabric prepared in Examples and Comparative Examples with distilled water, the total light transmittance was measured with a color computer measuring device of SUGA INSTRUMENT (Japan), and the results are shown in Table 3. Was

Total light transmittance (%) = (Specimen transmitted light)/(Specimen irradiated light)×100

[Table 3]

Referring to the results of Tables 2 to 3, the mask pack sheet products corresponding to Examples 1 to 5 show excellent results in water retention and transparency. On the other hand, the mask pack sheet products corresponding to Comparative Examples 1 to 5 show that it is impossible to maintain shape due to relatively low water retention and transparency or too high degree of substitution.

2 is a photograph of a CMC nonwoven fabric manufactured according to Example 4 of the present invention, and FIG. 3 is a photograph of a CMC nonwoven fabric manufactured according to Comparative Example 1 of the present invention. 2 and 3, FIG. 2 shows a transparent nonwoven, while FIG. 3 shows an opaque nonwoven.

As described above, the mask pack sheet product according to the present invention uses water and exhibits a carboxymethyl group substitution degree of 0.3 or less by controlling the concentration of the carboxymethylated solution. Accordingly, the mask pack sheet product exhibits high water retention and transparency, and at the same time maintains the shape required as a mask pack sheet product.

As described above with reference to the drawings illustrated for the present invention, the present invention is not limited by the embodiments and drawings disclosed in the present specification, and various by a person skilled in the art within the scope of the technical idea of the present invention. It is obvious that transformation can be made. In addition, even if not explicitly described and described the effects of the configuration of the present invention while describing the embodiments of the present invention, it is natural that the predictable effects of the configuration should also be recognized.

Claims (9)

Including a cellulose nonwoven fabric having a terminal substituted with a carboxymethyl group,
A mask pack sheet product with a degree of substitution of the carboxymethyl group of the cellulose nonwoven fabric from 0.05 to 0.3.
The method of claim 1,
The mask pack sheet product is a mask pack sheet product containing at least one ingredient exhibiting skin improvement functionality among moisturizing, soothing, elasticity, wrinkle improvement, and whitening.
(a) pretreating the cellulose nonwoven fabric by immersing it in an alkali solution;
(b) squeezing the pretreated cellulose nonwoven fabric;
(c) preparing a reaction solution by dissolving a carboxymethylating agent in water;
(d) adding the squeezed cellulose nonwoven fabric to the reaction solution, and substituting a hydroxy group at the end of the cellulose nonwoven fabric with a carboxymethyl group; And
(e) compressing and drying the substituted cellulose nonwoven fabric; Including,
In the step (d), a method of manufacturing a mask pack sheet product that is substituted to have a carboxymethyl group substitution degree of 0.05 to 0.3.
The method of claim 3,
In the step (a), the alkali solution has a concentration of 15 to 40%, and a method of manufacturing a mask pack sheet product that is pretreated at 20 to 70°C.
The method of claim 3,
A method of manufacturing a mask pack sheet product by squeezing so that the pickup rate of the cellulose nonwoven fabric with respect to the alkali solution in the step (b) is 200 to 500%.
The method of claim 3,
A method of manufacturing a mask pack sheet product in which a reaction solution is prepared by dissolving 20 to 60% by weight of a carboxymethylating agent in 40 to 80% by weight of water in step (c).
The method of claim 3,
The method of manufacturing a mask pack sheet product by mixing so that the weight ratio of the cellulose nonwoven fabric dehydrated in step (d): the reaction solution is 1: 2 to 1: 8.
The method of claim 3,
In the step (d), the substitution is performed at 70 to 150°C.
The method of claim 3,
In the step (e), drying is performed at 100 to 150°C.

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