KR20220005303A - A nano fiber dental mask and a method of manufacturing the same - Google Patents

Abstract

The present invention relates to a method for manufacturing a recyclable nanofiber-based dental mask. A recyclable nanofiber-based dental mask of the present invention to overcome the disadvantages of existing disposable masks by using traditional Korean paper and nanofibers consists of three layers of filters: a skin-friendly lining layer made of traditional Korean paper; a hydrophilic intermediate filter layer using nanofibers and impregnated nanoparticles; and a hydrophobic outer filter layer that is capable of self-cleaning and sterilizing by visible light, as well as diagnosis of environmental pollution exposure (e.g., air pollution, bacteria, virus, etc.).

Description

Nanofiber dental mask and manufacturing method thereof

The present invention relates to a skin-friendly traditional Korean paper that does not contain at least chemical components and a dental mask having a nanofiber layer laminated on the traditional Korean paper.

The present invention is provided with traditional Korean paper, an intermediate filter layer, and an outer filter layer, but at least the outer filter layer is hydrophobic to block dust, bacteria, and droplets, and the nanofiber layer of the present invention is a dispersed photocatalyst to prevent environmental pollution. It relates to a nanofiber dental mask that enables self-cleaning and sterilization and a method for manufacturing the same.

Korean traditional Korean paper has the best preservation and heat retention, antibacterial properties, far-infrared radiation, and deodorization properties for more than 1,000 years among the world's traditional tributary cultural properties.

Nanofibers mainly refer to fibers manufactured by electrospinning or an improved method. It is a method of manufacturing using the difference in charge, and it is in the spotlight as a technology that can manufacture ultrafine polymer fibers that cannot be processed by other methods. have. It is a relatively simple and easy method for producing fibers with nanometer to submicron diameters from solutions or melts of polymers, ceramics, composites, and metals. Electrospun ultrafine nanofibers have a much larger surface area than conventional ultrafine fibers, so they can be used as high-efficiency, ultra-functional filter materials that separate fine particles from gases or fluids, and the filtration efficiency of filtering small particles in the filter is improved. The heightening method is to use a fiber of an appropriate diameter in the filter medium, and nanofibers are known as the optimal material for this purpose.

Recently, research on materials with micro- and nanometer-sized structures for electrospun polymer fibers has been actively conducted, and these structures have a large specific surface area, a large surface area/volume ratio, and a porous structure. Due to the diffusion and easy penetration of electrolyte, it is widely applied to gas sensors, electrochemical cells (supercapacitors and secondary batteries), and various types of filters. Since the nanofibers produced by electrospinning are ultrafine fibers with a diameter of 1 μm or less, the fibrous filter removes contaminants from the air, such as diffusion effect, blocking effect, and electrostatic effect. The material may be removed.

Recently, the novel coronavirus infection (COVID-19) is spreading rapidly, but the 'mask crisis' shows no sign of being resolved, and the development of recycled materials is urgently needed. While the development of high-performance filter materials and the problem of fine dust are emerging, and interest in personal health is rapidly increasing, the filter industry for removing various pollutants is attracting attention, and research and market for high-performance fibers are expanding.

Accordingly, the present inventors came up with a triple filter dental mask including traditional Korean paper while proposing a dental mask for removing various contaminants while interest in personal health is rapidly increasing.

Prior literature: Korean Patent Publication No. 10-1130788 (Registered on March 20, 2012)

It is an object of the present invention to provide a nanofiber dental mask capable of preventing the adsorption and diffusion of environmental pollutants by being reusable as well as protecting users from environmental pollutants.

It is an object of the present invention to provide a nanofiber dental mask having a self-cleaning and self-sterilizing function for a dental mask contaminated with pathogens.

The dental mask of the present invention for achieving such a subject,

traditional hanji in which the inner surface is in contact with the wearer's skin;

A hydrophilic nanofiber layer laminated on the outer surface of the traditional Korean paper;

and a hydrophobic nanofiber layer provided on the outer surface of the hydrophilic nanofiber layer.

Preferably, the nanofiber dental mask,

(i) mounting the traditional Korean paper to the collector surface of the electrospinning machine as the mask endothelium in contact with the wearer's skin;

(ii) applying a high voltage between the electrospinning machine and the collector and spun nanofibers with a polymer solution by electrospinning to laminate an intermediate filter layer on the outer surface of traditional Korean paper;

(iii) electrospinning again on the outer surface of the nanofiber layer of the intermediate filter layer, but spinning the hydrophobic nanofibers with a hydrophobic polymer solution to laminate the outer filter layer;

Preferably, the intermediate filter layer is a hydrophilic polymer solution.

On the other hand, the polymer solution for spinning is impregnated with a photocatalyst so that the photocatalyst is dispersed in the nanofibers spun by electrospinning, so that it has self-cleaning and sterilization effects of pollutants by the reducing action of the photocatalyst under visible light.

The present invention is a nanofiber dental mask that can be manufactured by a simple manufacturing method and thus has excellent economic feasibility and can be reused while providing excellent hygiene, thereby minimizing group contamination.

The present invention provides a soft and comfortable touch because the surface that the wearer's skin touches becomes a gentle traditional Korean paper, and the outer filter layer of the nanofiber layer laminated on the traditional Korean paper is spun to make it hydrophobic and uses static electricity to , to prevent adsorption of dust, etc.

In the present invention, at least one of the intermediate filter layer and the outer filter layer is composed of a nanofiber layer in which a photocatalyst is dispersed. function is provided.

1 is a flowchart for a method of manufacturing a dental mask according to an embodiment of the present invention;
2 is a conceptual diagram of a nanofiber electrospinning device for manufacturing a triple filter;
_{3 is a graph showing the size and distribution of Ag-TiO 2} nanoparticles dispersed in a hydrophilic nanofiber layer by a TEM photograph after preparing them by hydrothermal synthesis;
4 is a schematic diagram of a photocatalyst and nanoparticle structure dispersed in a hydrophilic nanofiber layer
5 is an enlarged photograph of nanofibers in which a photocatalyst and nanoparticles are dispersed;
6 is a conceptual diagram of a photocatalytic action of a hydrophilic nanofiber.
Figure 7 is a photocatalyst and nanoparticles are dispersed hydrophilic nanofibers for antimicrobial activity against microorganisms
8 is a graph of experimental results in which methylene blue (MB) and (b) rhodamine B (RhB) solutions are photolysed by sunlight in the nanofiber layer.

Hereinafter, the present invention will be described in detail.

A dental mask with contamination diagnosis and sterilization functions manufactured in this way forms the following structure.

That is, a skin-friendly traditional Korean paper is provided as a base material in direct contact with the user's skin. A hydrophilic nanofiber layer is provided on the upper surface of the traditional Korean paper. And a hydrophobic nanofiber layer is provided on the upper surface of the hydrophilic nano-oil layer.

The manufacturing method of the nanofiber dental mask according to the present invention,

(S1) mounting the traditional Korean paper as a base material to the collector of the electrospinning machine;

- Simultaneously prepare the hydrophilic polymer solution and the hydrophobic polymer solution.

- Preferably, the polymer solution is from a polymer solution of PCL, PP, PE, PET, PLA, PLLA, PVDF, nylon 6, viscose, PU, PVA, PMMA, chitosan, Keratin fiber, cellulose fiber, pitch-based or PAN-based polymer. It is obtained by dissolving any one selected from sheep, silk, cotton, hemp, or recycled resources (hair, sheep, silk, cotton, hemp, ash, pulp), PAN fibers and pitch-based fibers.

- Carbon nanofibers prepared by stabilizing/charging nanofibers spun using the above polymer solution may be applied to the intermediate layer.

- Preferably, a photocatalyst and nanoparticles are dispersed in at least one polymer solution.

(S3) laminating a hydrophobic nanofiber layer as an outer filter layer by spinning a hydrophobic polymer solution by electrospinning on the surface of the inner filter layer of the traditional Korean paper;

- On the other hand, in the present invention, the hydrophobic nanofiber layer provided on the outermost surface blocks external droplets, dust, dust, etc. using static electricity.

As described above, a sufficient dental mask is prepared just by forming a hydrophobic nanofiber layer on traditional Korean paper.

However, preferably, the step (S2) of laminating an intermediate filter layer between (S1) and (S3) may be added. That is, an intermediate filter layer is provided between the traditional Korean paper and the hydrophobic outer filter layer, and the intermediate filter layer may be a hydrophobic intermediate filter or a hydrophilic intermediate filter.

- Preferably, the nanofibers of the intermediate filter layer adopt a hydrophilic polymer solution to absorb the traditional paper or microscopic particles or bacteria that have passed through the outer filter layer.

- Preferably, the nanofiber spinning step for the intermediate filter layer is sufficiently laminated on the surface of the traditional Korean paper through several times of electrospinning, so that foreign substances are filtered out once more by the fine fiber structure by the fine fiber structure.

As described above, by laminating the surface of traditional Korean paper with nanofibers, it is possible to make a mask of a double or triple filter. In the dental mask of the present invention, it is possible to integrally form nanofiber radiation layer-by-layer, that is, layer by layer by one process.

2 is a conceptual diagram of electrospinning for manufacturing the nanofiber dental mask of the present invention. Based on traditional Korean paper with high skin-friendly and antibacterial and deodorizing properties, electrospinning a polymer solution impregnated with nanoparticles and photocatalysts (hydrophilic or hydrophobic) to laminate an intermediate filter layer with excellent breathability and water resistance, and then use a hydrophobic polymer solution. The outer filter layer is laminated by direct spinning of the hydrophobic nanofiber. The outer filter layer with hydrophobicity filters out dust, dust, and droplets by using static electricity, and filters out environmental pollutants first.

In the hydrophilic or hydrophobic polymer solution, a photocatalyst and nanoparticles are introduced and dispersed together on the surface of the spun nanofiber. Photocatalyst is a kind of catalyst and refers to a semiconductor material that decomposes various bacteria and pollutants by accelerating the catalytic reaction (oxidation-reduction reaction) using light as an energy source due to the catalytic action of the photocatalyst. In other words, when photocatalyst particles are put into a solution and irradiated with energy light greater than the band gap, electrons having a negative charge and holes having a positive charge are generated, and the strong reduction or oxidation action decomposes the ionic or molecular species in the solution. provokes various reactions. Materials that can be used for the photocatalyst include TiO ₂ (anatase), TiO ₂ (rutile), ZnO, CdS, ZrO ₂ , V ₂ O ₃ , WO _{3 ,} and perovskite-type composite metal oxide (SrTiO ₃ ). The photocatalyst dispersed in the polymer solution is typically TiO ₂ is preferred. TiO ₂ itself does not change even when exposed to light, so it can be used semi-permanently. ZnO and CdS, which have excellent effects on the decomposition of trichlorethylene and tetrachlorethylene, absorb light, so that the catalyst itself is decomposed by light, generating harmful Zn and Cd ions. In addition, TiO ₂ oxidizes all organic materials and decomposes to carbon dioxide and water, but WO ₃ has good efficiency as a photocatalyst only for specific substances, and other than that, the efficiency is _{not as good as TiO 2} , so the usable area is very limited.

Since such a nanofiber dental mask can be sterilized, it can be recycled compared to a conventional dental mask, thereby providing the best means for preventing infectious diseases.

<Example 1>

Manufacturing method of laminated triple filter by single process

Step 1: Preparing traditional Korean paper and mounting it on the collector of the electric spinning machine;

_{Step 2: The Ag-TiO 2} nanoparticles are impregnated on traditional paper under the conditions of Tip-to Collector Distance 15 cm, Voltage 15 kV, temperature and humidity 25 ± 2℃ / 50 ±2 %, and feeding rate 0.1ml/min. After spinning polyurethane nanofibers using the hydrophilic polyurethane (PU), laminating a predetermined thickness;

Step 3: Continuously spinning and laminating hydrophobic polyvinylidene fluoride (PVDF) in a spider-net structure on the upper surface of the polyurethane nanofiber layer; through,

A nanofiber dental mask is manufactured using traditional Korean paper as the inner skin filter layer and having a triple filter of a hydrophilic intermediate filter layer and a hydrophobic outer layer filter layer.

<Example 2>

Manufacturing method of triple filter including carbonization process

Step 1: After spinning PAN nanofibers under the conditions of Tip-to Collector Distance 15 cm, Voltage 15 kV, temperature and humidity 25 ± 2 ℃ / 50 ± 2 %, and feeding rate 0.1ml/min, heating rate 5 ℃/ After stabilizing at 240 °C for 30 minutes at min, producing carbon nanofibers through a carbonization process at 850 °C for 4 hours at a heating rate of 5 °C/min;

- Although it is preferable to spin PAN-based nanofibers, it is not necessary to limit to PAN-based nanofibers.

Step 2: The carbon nanofibers and traditional Korean paper prepared in step 2 are laminated with each other.

- The traditional Korean paper preferably has a high density/high strength basis weight of 200 g/m 2 or less.

Step 3: Including the step of laminating by spinning nylon 6 in a spider-net structure on the basis of the mat made in step 2,

Using traditional Korean paper as the inner skin layer, a nanofiber dental mask is manufactured in the triple filter of the hydrophobic intermediate filter layer and the hydrophobic outer filter layer.

On the other hand, in the present invention, using traditional Korean paper as the inner skin layer and spinning a polymer solution to laminate nanofibers, electrospinning an eco-friendly polymer solution impregnated with a photocatalyst and nanoparticles to obtain a structure in which the photocatalyst is dispersed on the surface of the nanofiber can ㅇ In addition to the photocatalyst, nanoparticles such as fly ash, carbon quantum dots, and gC ₃ N ₄ may be introduced and dispersed together in the nanofiber.

The nanofiber layer sprayed with the photocatalyst can be self-cleaning by visible light, and it becomes possible to sterilize environmental pollution (air/bacteria, virus).

Accordingly, due to the sterilization effect under visible light as well as ultraviolet light, it has a remarkable effect to prevent group infection even in an enclosed space.

4 and 5 are schematic diagrams illustrating the structure when a photocatalyst and nanoparticles are introduced and dispersed on the surface of the nanofiber based on the result of [Fig. 3] above to the nanofiber of the present invention. Nanofibers in which the photocatalyst is dispersed can self-clean and sterilize contaminants by photocatalysis in ultraviolet and visible light.

6 is a conceptual diagram for the photocatalytic action experiment of the intermediate filter layer nanofiber of [FIG. 4] of the present invention. When exposed to environmental pollutants and infected with viruses or microorganisms, it is a mechanism that immediately sterilizes and removes pollutants by ultraviolet or visible light.

7 is a result of testing the antimicrobial properties of the nanofibers impregnated with the photocatalyst and nanoparticles in FIG. 6 against microorganisms. (a)(c) shows the antibacterial properties of E. coli and S. aureus of _{polyacrylonitrile (PAN) nanofibers and PAN nanofibers impregnated with Ag 3} PO _{4 .}

(b)(d) shows the antibacterial properties of E. coli and S. aureus of polyacrylonitrile (PAN) nanofibers and Ag ₃ PO _{4 /PAN nanofibers introduced with SO 4} ^2-.

In addition, (e)(f) shows the antibacterial properties of E. coli and S. aureus of Ag ₃ PO _{4 /PAN nanofibers introduced with polyacrylonitrile (PAN) nanofibers and SO 4} ^{2- in the dark.} .

As a result of the experiment, pure PAN nanofibers did not show antibacterial properties, but Ag ₃ PO ₄ impregnated PAN nanofibers and SO ₄ ^2- introduced Ag ₃ PO ₄ /PAN nanofibers were in the order of E. coli and S. aureus. antibacterial activity was increased. But in the dark there was no reaction. It was confirmed that the tested dental mask made of nanocomposite material showed a sterilization reaction by sunlight.

8 is an experimental result in which methylene blue (MB) and (b) rhodamine B (RhB) solutions are photolysed by normal sunlight in a nanofiber layer impregnated with a photocatalyst and nanoparticles in the present invention. i) PAN nanofibers, ii) PAN-based carbon nanofibers impregnated with CdSe, or iii) PAN-based carbon nanofibers impregnated with Co and CdSe are spun, respectively, and vacuum dried at 70°C for 12 hours, followed by 2 at 250°C. As a result of examining the photodegradation reaction according to time of carbon nanofibers subjected to time stabilization process and carbonization process at 800℃ for 2 hours, PAN-based carbon nanofiber < PAN-based carbon nanofiber impregnated with CdSe < Co and CdSe impregnated together It was found that the photolysis effect increased in the order of PAN-based carbon nanofibers.

100: electric thrower
200 : Collector
300: traditional Korean paper
400: intermediate filter layer
500: outer filter layer

Claims (8)

Traditional Korean paper 300 with the inner surface in contact with the wearer's skin;
Nanofiber dental mask, characterized in that the outer filter layer 500 is laminated on the outer surface of the traditional Korean paper, the outer filter layer 500 is a hydrophobic nanofiber layer.
According to claim 1,
An intermediate filter layer 400 laminated by the nanofibers spun by the electrospinning machine 100 between the outer surface of the traditional Korean paper 300 and the hydrophobic nanofiber layer 500 is further provided, the intermediate filter layer 400 Nanofiber dental mask, characterized in that the silver hydrophilic nanofiber layer.
3. The method of claim 2,
Nanofiber dental mask, characterized in that the photocatalyst is impregnated in the polymer solution that is spun into the intermediate filter layer or the outer filter layer and laminated so that the photocatalyst is dispersed on the surface of the nanofiber by electrospinning.
4. The method of claim 3,
The photocatalyst is TiO _2, and nanofiber dental mask, characterized in that at least one selected from ZnO.
5. The method according to claim 3 or 4,
Nanofiber dental mask, characterized in that the polymer solution is _{introduced together with the photocatalyst and nanoparticles of gC 3} N ₄ , fly ash or carbon quantum dots to promote photocatalysis in the nanofiber layer.
5. The method according to claim 3 or 4,
The nanofiber dental mask, characterized in that the hydrophobic polymer solution for the outer filter layer is hydrophobic polyvinylidene fluoride (PVDF).
(i) mounting the traditional Korean paper on the collector surface of the electrospinning machine;
(ii) applying a high voltage between the electrospinning machine and the collector and spinning a hydrophilic polymer solution by electrospinning to laminate a hydrophilic nanofiber layer on the outer surface of traditional Korean paper;
(iii) spinning a hydrophobic polymer solution by electrospinning again on the outer surface of the hydrophilic nanofiber layer to laminate a hydrophobic nanofiber layer; nanofiber dental mask manufacturing method manufactured by a manufacturing method comprising a.
- spinning a nanofiber by spinning a PAN-based polymer solution; (W1)
- The nanofiber is manufactured into carbon nanofibers through a carbonization process; (W2)
- Laminating the carbon nanofibers and traditional Korean paper produced by step (W2); (W3)
- Laminating by spinning nylon 6 in a spider-net structure on the outer surface of the carbon nanofiber on the basis of the carbon nanofiber and traditional Korean paper mat made in step (W3); (W4) including,
A method of manufacturing a nanofiber dental mask with a triple filter of a hydrophobic intermediate filter layer and a hydrophobic outer filter layer using traditional Korean paper as the inner skin layer.

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