KR20210086795A - Manufacturing method of natural plant extract coated filter having for its own antibacterial - Google Patents

Abstract

The present invention relates to a method for manufacturing an antibacterial filter, and more specifically, to a method for manufacturing a natural substance-coated filter having antibacterial properties by itself by applying an antibacterial solution containing a natural substance on the surface of a filter and drying the solution. To this end, the method for manufacturing an antibacterial filter includes: a first step of manufacturing a silica precursor solution by mixing a silica precursor and distilled water; a second step of aging by adding an acid to the silica precursor solution and stirring the solution; a third step of manufacturing an antibacterial solution by adding a natural antibacterial material to the aged silica precursor solution and stirring the solution; and a fourth step of coating by applying the antibacterial solution to the surface of an object to be coated.

Description

Manufacturing method of natural product coating filter having its own antibacterial properties {MANUFACTURING METHOD OF NATURAL PLANT EXTRACT COATED FILTER HAVING FOR ITS OWN ANTIBACTERIAL}

The present invention relates to a method for manufacturing an antibacterial filter, and more particularly, to a method for manufacturing a natural product-coated filter having antibacterial properties by applying and drying an antibacterial solution containing a natural product on the filter surface.

Recently, as interest in fine dust and the environment increases, the demand for improving indoor air quality is increasing. Various microorganisms such as viruses, bacteria, and bacteria are suspended in the air, and these suspended microorganisms cause infectious diseases and various respiratory and skin diseases. Therefore, filters that can remove these microorganisms are installed in air purifiers, air conditioners, automobiles, HVAC (Heating, Ventilation, and air-conditioning) systems, etc. is being used

In particular, since various microorganisms can breed on the surface of the filter from which various contaminants are filtered, and secondary contamination occurs accordingly, an antibacterial filter having antibacterial properties in the filter itself is being developed to antibacterially and sterilize these microorganisms.

In Korea Patent Publication No. 10-0321589 and Korean Patent Publication No. 10-0455664, metal ions such as silver and iodine, which have excellent antibacterial properties, are used as inorganic antibacterial substances in activated carbon, chemicals, or carriers such as silica, alumina, and zeolite. Although it has the advantage of long lasting antibacterial activity, some metals are toxic to the human body and have the disadvantage of causing environmental pollution, so their application as an antibacterial material is limited. Organic antibacterial substances can be divided into synthetic compounds and natural antibacterial agents. Although synthetic compounds have excellent antibacterial properties, they are not used as antibacterial substances due to lack of stability to the human body.

In Korean Patent Publication No. 10-0094495 and Korean Patent Publication No. 10-0054144, grapefruit extract and propolis are used as natural antibacterial substances to give antibacterial properties, and there are no side effects to the human body and problems such as inducing environmental pollution Although propolis is an expensive natural material, it is difficult to apply to mass production, and grapefruit extract has a disadvantage in that antibacterial properties are somewhat lower.

Republic of Korea Patent Publication No. 10-0131288

The present invention is to solve the above problems, and an object of the present invention is to provide a method of manufacturing a natural product-coated filter having antibacterial properties by applying and drying an antibacterial solution containing a natural product on the filter surface.

These and other objects and advantages of the present invention will become apparent from the following description of preferred embodiments.

The above object, a first step of preparing a silica precursor solution by mixing a silica precursor and distilled water; A second step of aging by adding an acid to the silica precursor solution and then stirring; A third step of preparing an antibacterial solution by adding a natural antibacterial material to the aged silica precursor solution and stirring; and a fourth step of coating the surface of the object to be coated by applying the antibacterial solution to the surface of the object to be coated.

The silica precursor of the first step may be tetramethyl orthosilicate (TMOS).

In the second stage of aging, after adding acid, sonication is performed for 5 to 20 minutes, and aging can be performed at 3 to 5 ° C. for 10 to 15 hours. At this time, the acid may be hydrochloric acid. have.

The natural antibacterial substance of the third step may be tea tree oil, rosemary extract or garlic extract.

The fourth step may use a spray coating method, and specifically, a 4-1 step of applying an antibacterial solution to the surface of the object to be coated using a spray coating method; and a 4-2 step of drying the antibacterial solution applied to the surface of the object to be coated.

In this case, a sol thin film may be formed on the surface of the object to be coated in step 4-1, and the sol thin film may be dried in step 4-2 to form a gel thin film.

According to the present invention, it is possible to provide an antibacterial filter that is harmless to the human body and has excellent antibacterial properties.

Specifically, it is possible to provide an antibacterial filter that replaces conventional antibacterial agents by exhibiting excellent antibacterial properties against harmful bacteria or bacteria such as Micrococcus luteus, the causative agent of pneumonia and meningitis, and E. coli, Staphylococcus aureus, and pneumococcus among bacteria floating in the air. have.

In addition, unlike the UV lamp, photocatalyst, plasma, or ozone method, it does not require a separate power supply, so it can have an effect that can be applied to various products.

However, the effects of the present invention are not limited to the above-mentioned effects, and other effects not mentioned will be clearly understood by those skilled in the art from the following description.

1 is an image of the surface of Example 1 observed with a scanning electron microscope.
2 is an image of a surface of a comparative example observed with a scanning electron microscope.
3 is a graph showing the pressure loss of Examples 1 to 3;
4 to 6 are graphs showing the antimicrobial activity against M. luteus (+) bacteria of Examples 1-3.
7 to 8 are views showing the state 18 hours after pneumococcal inoculation for the filters of Examples 1 to 3 and Comparative Examples. 7 is a view showing a comparative example (top) and Example 1 (bottom), and FIG. 8 is a view showing Example 2 (top) and Example 3 (bottom).
9 to 10 are views showing the state 18 hours after Staphylococcus aureus inoculation for the filters of Examples 1 to 3 and Comparative Examples. Fig. 9 is a view showing a comparative example (top) and Example 1 (bottom), and Fig. 10 is a view showing Example 2 (top) and Example 3 (bottom).

Hereinafter, the present invention will be described in detail with reference to embodiments and drawings of the present invention. It will be apparent to those of ordinary skill in the art that these examples are merely presented by way of example to explain the present invention in more detail, and that the scope of the present invention is not limited by these examples. .

Further, unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and in case of conflict, this specification, including definitions description will take precedence.

In order to clearly explain the invention proposed in the drawings, parts irrelevant to the description are omitted, and similar reference numerals are attached to similar parts throughout the specification. And, when a part "includes" a certain component, this means that other components may be further included, rather than excluding other components, unless otherwise stated. In addition, "unit" described in the specification means one unit or block that performs a specific function.

In each step, the identification number (first, second, etc.) is used for convenience of description, and the identification number does not describe the order of each step, and each step does not clearly describe a specific order in context. It may be performed differently from the order specified above. That is, each step may be performed in the same order as specified, may be performed substantially simultaneously, or may be performed in the reverse order.

A first step of preparing a silica precursor solution by mixing the silica precursor and distilled water according to an embodiment of the present invention; A second step of aging by adding an acid to the silica precursor solution and then stirring; A third step of preparing an antibacterial solution by adding a natural antibacterial material to the aged silica precursor solution and stirring; and a fourth step of coating by applying the antibacterial solution to the surface of the object to be coated.

The present invention forms a coating layer containing a natural antibacterial material, such as a natural plant extract, on the surface of a filter such as a nonwoven fabric, so that among bacteria floating in the air, Micrococcus luteus, the causative agent of pneumonia and meningitis, and Escherichia coli, Staphylococcus aureus, pneumococcus, etc. It is a filter manufacturing method that exhibits excellent antibacterial properties against harmful bacteria or bacteria. The antibacterial filter manufactured through the present invention does not require a separate power supply unlike the UV lamp, photocatalyst, plasma, or ozone method, so it can be applied to various products, which can replace conventional antibacterial agents. have

The first step is a step of preparing a silica precursor solution by mixing a silica precursor and distilled water. The silica precursor solution is finally formed in the form of a gel on the surface of the object to be coated and functions as a support for supporting the antibacterial material. As the silica precursor, various known materials can be used, but it is preferable to use tetramethyl orthosilicate (TMOS) in order to prepare an effective gel form. In addition, it is preferable to mix tetramethyl orthosilicate and distilled water in a ratio of 1:1 in order to improve the antibacterial material loading efficiency.

The second step is a step of aging by stirring after adding an acid to the silica precursor solution. In this case, various known acids may be added, but it is preferable to use 0.2 M hydrochloric acid. Specifically, after adding an acid to the silica precursor solution, sonication may be performed for 5 to 20 minutes, and aging may be performed at 3 to 5° C. for 10 to 15 hours. For example, 0.2 M hydrochloric acid is added to the silica precursor solution, followed by sonication for 10 minutes, and aging at 4° C. for 12 hours.

The third step is to prepare an antibacterial solution by adding and stirring a natural antibacterial material to the aged silica precursor solution, and the natural antibacterial material is a concept including various antibacterial substances derived from nature, such as natural plant extracts.

In one embodiment, the natural antibacterial substance may be tea tree oil.

Tea tree oil is called melaleuca oil and can be made from the tea tree leaves. Tea tree oil can be prepared in a form that is very clear or has a slightly pale golden or yellow scent with fresh camphor. Tea tree oil has strong antifungal, antibacterial and antiviral properties and is also used in dental and surgical treatments. Tea tree oil can be produced through various distillation methods, but is preferably produced through steam distillation method.

In one embodiment, the natural antibacterial substance may be a rosemary extract.

Rosemary is native to the Mediterranean coast of southern Europe. It is a herb plant with a strong scent of Lamiaceae and is also called Mijilyang. The extract of rosemary is used as a fragrance in cosmetics and soaps, as a skin conditioning agent, and as a moisture barrier agent. The rosemary extract can be prepared through various methods, but it can be prepared by grinding rosemary leaves, extracting them with 80-100% alcohol at a temperature of 25-40° C. for 24 hours, and then concentrating.

In one embodiment, the natural antibacterial substance may be a garlic extract.

Garlic extract is a component extracted from the scales of garlic and is rich in protein, vitamins B1, B2, C, glutamic acid, calcium, iron, phosphorus, zinc and selenium. In general, garlic extract is used in cosmetics because it can inhibit the activity of external substances that adversely affect the skin, but when applied to a filter as in the present invention, an effective antibacterial effect can be obtained. Garlic extract may be extracted by crushing garlic, but it is preferable to extract after mixing various additives in order to improve the antibacterial effect of garlic extract. In this case, the additive may include bee pollen, barley sprout powder and cheongung powder.

Bee pollen is a solid mass made by mixing bees' saliva with pollen collected by bees from flowers. It is widely known as a complete food as an essential nutrient for bees to raise larvae, and is called Bee Pollen. Efficacy of bee pollen has also been recorded in Donguibogam decoction, and contains 20 kinds of amino acids, 16 kinds of natural vitamins, and 17 kinds of minerals. Bee pollen can be mixed with garlic powder to enhance its antibacterial effect. Bee pollen can be used by mixing 10 to 20 parts by weight based on 100 parts by weight of garlic. When the bee pollen is less than 10 parts by weight based on 100 parts by weight of garlic, the effect is insignificant, and when it exceeds 20 parts by weight, there is a concern that the concentration of the extract may be lowered during extraction at high temperature.

Sprout barley powder is harvested, dried and powdered after planting barley seeds for 10 days. Sprout barley powder makes it possible to effectively extract the active ingredient inside garlic, and is preferably included in an amount of 1 to 5 parts by weight based on 100 parts by weight of garlic. If the content of the sprouted barley powder is less than 1 part by weight, it is difficult to express the desired extraction effect, and if it exceeds 5 parts by weight, it is uneconomical because it only causes consumption of raw materials without an additional extraction effect.

Chunkyung powder is a perennial plant of the Dicotyledonous plant, Dicotyledonous family, Umbilicalaceae family, and it is powdered after digging up the rhizomes, removing the leaves and stems, and drying them in the sun. Chunkyung powder has an antibacterial effect that can suppress the activity of pathogenic fungi such as cholera. Cheongoong powder is preferably included in 3 to 5 parts by weight based on 100 parts by weight of garlic. When the content of Chunkyung powder is less than 3 parts by weight, the antibacterial action due to Chunkyung is insignificant, and when it exceeds 5 parts by weight, there is a problem in that too strong a scent is emitted.

Specifically, after crushing garlic with a blender, 10 to 20 parts by weight of bee pollen, 1 to 5 parts by weight of sprouted barley powder, and 3 to 5 parts by weight of cheongung powder are added with respect to 100 parts by weight of garlic, and 1000 parts by weight (of garlic) After adding 10 times) of water, it can be extracted by heating at 90 to 100° C. for 3 to 5 hours using a reflux condenser.

The fourth step is a step of coating by applying the antimicrobial solution to the surface of the object to be coated, and the antibacterial solution may be applied to the surface of the object to be coated by using a spray method. Specifically, the 4-1 step of applying the antibacterial solution to the surface of the object to be coated using a spray coating method; and a 4-2 step of drying the antibacterial solution applied to the surface of the object to be coated; in the 4-1 step, the antibacterial solution is primarily formed in the form of a sol thin film, and in the 4-2 step The sol thin film is dried to form a gel thin film.

For example, the antibacterial solution is directly sprayed on the surface of the air filter in the form of a nonwoven fabric and applied through a spray coating method to form a sol thin film layer, and when the sol thin film layer dries, a gel thin film layer with a number of micropores is formed to effectively support the antibacterial material. can do. As the supported antibacterial material is gradually diffused outward, the antibacterial filter can perform an antibacterial function for a long time.

Hereinafter, the configuration of the present invention and its effects will be described in more detail through specific examples and comparative examples. However, these examples are for explaining the present invention in more detail, and the scope of the present invention is not limited to these examples.

[Example 1: Tea-tree oil]

A silica precursor solution was prepared by mixing 20 ml of tetramethyl orthosilicate and 20 ml of distilled water. Then, 0.2M hydrochloric acid 2.64ml was added, followed by sonication at room temperature for 10 minutes, and aging at 4°C for 12 hours. Thereafter, 8.534 ml of tea tree oil was mixed as a natural antibacterial material and stirred to prepare an antibacterial solution. The antibacterial solution was applied to the nonwoven fabric of the air filter by spray coating and dried at room temperature for 12 hours to prepare an antibacterial filter.

[Example 2: Rosemary]

An antibacterial filter was prepared in the same manner as in Example 1, except that rosemary extract was used instead of tea tree oil as a natural antibacterial material.

[Example 3: Garlic]

An antibacterial filter was prepared in the same manner as in Example 1, except that garlic extract was used instead of tea tree oil as a natural antibacterial material.

At this time, 100 parts by weight of garlic extract was pulverized with a blender, then 15 parts by weight of bee pollen, 3 parts by weight of sprouted barley powder, and 4 parts by weight of cheongung powder were added, 1000 parts by weight of water was added, and then 90 parts by weight using a reflux cooler. It was extracted by heating at ℃ for 3 hours.

[Comparative example]

An antibacterial filter was prepared in the same manner as in Example 1, except that a natural antibacterial material was not used.

[Experimental Example 1: Surface observation]

The antibacterial filters of Example 1 and Comparative Examples were observed with a scanning electron microscope, and are shown in FIGS. 1 and 2 . In the case of Figure 1, it can be seen that the coating layer is formed on the surface of each fiber component of the nonwoven fabric because the antibacterial material is coated. In particular, when the coating solution is agglomerated, it can be seen that the coating layer is agglomerated and the actual coating layer is formed. represents the surface of 1, it was confirmed that the tea tree oil was supported on the nonwoven fabric.

[Experimental Example 2: Pressure loss test]

3 is a graph comparing the pressure loss of the filters coated with each natural antibacterial material in the antibacterial filters of Examples 1 to 3; Example 1 (Tea-tree oil) when the pressure loss was measured at approximately 0.2mmH ₂ O Example 2 (Rosemary) substantially 0.19mmH for approximately 0.16mmH ₂ O was measured in Example 3 (Garlic) For Measured as _{2 O.} In the case of the air filter, when the air permeability is weakened by the coating, the air purification ability is remarkably lowered, but it was confirmed that Examples 1 to 3 did not generate almost any pressure loss and thus were suitable for the material for the air filter.

[Experimental Example 3: Antibacterial test - M. luteus (+) bacteria]

M. luteus (+) bacteria were sprayed on the antibacterial filter of Examples 1 to 3 for 2 minutes and collected on the filter surface. Each antibacterial filter was coated according to the concentration according to the natural antibacterial material. The bacteria collected in each antibacterial filter were extracted by putting each antibacterial filter in 30 ml of distilled water, and performing a vortexing process for 2 minutes.

The extract obtained through the above-described process was diluted and spread on an agar plate by 100 ul, and after culturing for 48 hours at a temperature of 37 ° C in an incubator, their colony forming units (CFU) were measured. .

4 to 6 are graphs schematically showing the specific activity of microorganisms according to the concentration of natural antibacterial substances in the antibacterial filters of Examples 1 to 3; At this time, the control (control) is nothing is put, the coating solution (coating solution, comparative example) is a natural antibacterial substance is not put. In the case of Example 1 (FIG. 4), the antibacterial properties of 99.65% and 99.97%, respectively, were exhibited at the concentrations of 1% and 5%, and the antibacterial properties of 99.99% were exhibited at the concentration of 10% or more. In the case of Example 2 (FIG. 5), it was confirmed that a maximum of 98.97% antibacterial activity was shown, and in the case of Example 3 (FIG. 6), a maximum of 99.99% of the antibacterial activity was shown.

[Experimental Example 4: Antimicrobial Test - Pneumococcus ( Klebsiella pneumonae ATCC 4352) and Staphylococcus aureus ATCC 6538]

For the antibacterial filters of Examples 1 to 3, the antibacterial properties were measured. At this time, Example 1 used an antibacterial filter containing 20% tea tree oil, Example 2, 20% rosemary extract, and Example 3, 50% garlic extract.

Specifically, according to the KS K 0693:2016 method, the pneumococcus ( Klebsiella pneumonae ATCC 4352) inoculation liquid and Staphylococcus aureus ATCC 6538) inoculation bacterial liquid were inoculated into the medium, respectively, and then, each of Examples 1 to 3 were inoculated on the upper side of the medium. After attaching the filter and the filter of Comparative Example, bacteria were cultured for 18 hours.

After 18 hours, the number of remaining bacteria was compared to measure the removal rate of pneumococcus and Staphylococcus aureus. As a result, the filter of Comparative Example propagated pneumococcus and Staphylococcus aureus, but the antibacterial filters of Examples 1 to 3 were used for pneumonia. It was confirmed that more than 99.99% of cocci and Staphylococcus aureus were removed.

In this specification, only a few examples among the various embodiments performed by the present inventors are described, but the technical spirit of the present invention is not limited or limited thereto, and it is of course that it may be modified and variously implemented by those skilled in the art.

Claims (10)

A first step of preparing a silica precursor solution by mixing a silica precursor and distilled water;
A second step of aging by adding an acid to the silica precursor solution and then stirring;
A third step of preparing an antibacterial solution by adding a natural antibacterial material to the aged silica precursor solution and stirring; and
A method of manufacturing an antibacterial filter comprising a; a fourth step of coating the surface of the object to be coated with an antibacterial solution. According to claim 1, wherein the silica precursor of the first step,
Tetramethyl orthosilicate (TMOS, tetramethyl orthosilicate), characterized in that, the manufacturing method of the antibacterial filter. According to claim 1, Aging in the second step,
After the acid is added, sonication is performed for 5 to 20 minutes, and aging at 3 to 5° C. for 10 to 15 hours, a method of manufacturing an antibacterial filter. 4. The method of claim 3, wherein the acid is
A method of manufacturing an antibacterial filter, characterized in that it is hydrochloric acid. According to claim 1, wherein the natural antibacterial material of the third step,
A method of manufacturing an antibacterial filter, characterized in that tea tree oil. According to claim 1, wherein the natural antibacterial material of the third step,
A method for producing an antibacterial filter, characterized in that it is a rosemary extract. According to claim 1, wherein the natural antibacterial material of the third step,
A method of manufacturing an antibacterial filter, characterized in that it is a garlic extract. According to claim 1, wherein the fourth step,
A method of manufacturing an antibacterial filter, characterized in that using a spray coating method. According to claim 1, wherein the fourth step,
Step 4-1 of applying the antibacterial solution to the surface of the object to be coated using a spray coating method; and
A method of manufacturing an antibacterial filter, comprising: drying the antimicrobial solution applied to the surface of the object to be coated; 10. The method of claim 9,
In step 4-1, a sol thin film is formed on the surface of the object to be coated,
The method for manufacturing an antibacterial filter, characterized in that the sol thin film is dried in step 4-2 to form a gel thin film.

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