KR20080084337A - Anti-microbial coating composition and use thereof - Google Patents

Abstract

An antibacterial coating composition, a method for preparing the composition, a filter paper coated with the composition, and a deodorizing filter containing the filter paper are provided to allow the antibacterial or fungicidal component to be released steadily from a microcapsule for a long time. An antibacterial coating composition comprises 15-25 wt% of an antibacterial microcapsule; and 75-85 wt% of a binder mixture. Preferably the antibacterial microcapsule comprises an antibacterial core; and a melamine resin, a urea resin, an acrylic resin or their mixture which is coated on the core. Preferably the binder mixture comprises 30-45 wt% of ethyl acrylate; 0.5-1.5 wt% of N-methylol acrylamide; 0.1-1 wt% of ammonium persulfate; 0.5-1.5 wt% of ammonium hydroxide; 1-2 wt% of methacrylic acid; and 20-70 wt% of a solvent.

Description

Antimicrobial Coating Composition and Use Thereof

1 is a block diagram of a deodorizing filter including a filter filter coated with an antimicrobial coating liquid composition according to the present invention;

Figure 2 is a view showing the antimicrobial test results of the deodorizing filter according to Example 5 of the present invention,

Figure 3 is a view showing the antimicrobial test results of the deodorizing filter according to Comparative Example 1 of the present invention,

Figure 4 is a view showing the antimicrobial test results of the deodorizing filter according to Comparative Example 2 of the present invention,

5 is a view showing the anti-mildew test results of the deodorizing filter according to Example 5 of the present invention,

Figure 6 is a view showing the anti-mildew test results of the deodorizing filter according to Comparative Example 1 of the present invention,

7 is a view showing the anti-mildew test results of the deodorizing filter according to Comparative Example 2 of the present invention.

The present invention relates to an antimicrobial coating liquid composition and its use, and more particularly, to an antimicrobial coating liquid composition comprising an antimicrobial microcapsules microencapsulated antibacterial and / or air palm isomers and its use.

A general deodorization filter is a filter used in an air conditioner such as an air purifier, a household or a vehicle air conditioner or a ventilation fan, and has activated carbon as an adsorbent material therein to adsorb odors and bacteria. However, since odors and bacteria are adsorbed at the adsorption point of activated carbon, deodorization performance decreases after all the odors and bacteria are adsorbed, and there are problems such as bacteria or mold propagation inside the filter.

Thus, some of the deodorizing filter was manufactured using a silver or antimicrobial treatment, such as antibacterial filter, but an example of applying the anti-mildew treatment can not be found.

Since the main cause of the smell and contamination of the deodorant filter is the mold, anti-mildew treatment may be essential in the manufacture of the deodorant filter. When a certain time elapses, most of the antimicrobial substances are adsorbed on the activated carbon, thereby degrading the antimicrobial performance.

On the other hand, the application of the antimicrobial agent for the antibacterial and antifungal treatment of the deodorizing filter can be largely divided into solid type and liquid type bar, when the same antimicrobial agent is applied at the same concentration, the liquid type is more eluted and diffused than the solid type type This is excellent and shows better antibacterial and / or antifungal performance.

However, the liquid type antimicrobial agent is not easy to handle and has a problem in that it is easily eluted and diffused so that the persistence of antibacterial and / or antifungal performance is short.

Thus, in order to continuously exhibit antibacterial and / or antifungal performance over a long time, it is necessary to microencapsulate the antimicrobial material to control the release rate of the antimicrobial material.

The present invention is to solve the above problems, there is a technical problem to provide an antimicrobial coating liquid composition comprising an antimicrobial microcapsules containing an antibacterial material having antibacterial and / or anti-fungal.

In addition, the present invention has a technical problem to provide a filter filter coated with the antimicrobial coating liquid composition or a deodorizing filter including the filter filter.

In addition, the present invention provides a method for producing an antimicrobial coating liquid composition comprising the antimicrobial microcapsules.

In one aspect, the present invention provides an antimicrobial coating liquid composition comprising 15 to 25% by weight of the antimicrobial microcapsules and 75 to 85% by weight of the binder mixture relative to the total coating liquid weight.

In another aspect, the present invention comprises the steps of mixing 2 to 6% by weight of the dispersant per 30% by weight of the total reactant to 30 to 40% by weight of the solvent, followed by stirring for 20 to 40 minutes at a temperature of 60 to 90 ℃; 30 to 40% by weight of the solvent is further mixed with the cooled mixture, followed by adding 15 to 25% by weight of the antimicrobial substance, followed by stirring at 1,500 to 1,900 rpm; 2 to 5% by weight of monomer and 3 to 6% by weight of formalin were added to the stirred mixture to form the outer wall of the microcapsules, followed by polymerization at 500 to 600 rpm for 3 to 4 hours at a temperature of 50 to 80 ° C. To prepare a microcapsule slurry; And it provides a method for producing an antimicrobial coating liquid composition comprising mixing 15 to 25% by weight of the antimicrobial microcapsules relative to the total coating liquid weight with a binder mixture of 75 to 85% by weight relative to the total coating liquid weight.

In another aspect, the present invention provides a filter filter coated with an antimicrobial coating liquid composition and a deodorizing filter including the filter filter.

Here, the binder mixture constituting the antimicrobial coating solution composition is 30 to 45% by weight of ethyl acrylate, 0.5 to 1.5% by weight of N-methylol acrylamide, 0.1 to 1% by weight of ammonium persulfate, 0.5 to 1.5% by weight of ammonium hydroxide %, Methacrylic acid 1-2% and solvent 50-70% by weight.

The antimicrobial material according to the present invention is an antibacterial and / or antifungal substance, and any antimicrobial and / or antifungal substance may be used, but preferably 2-n-octyl-4. It is recommended to use isothiazolin-3-one (OIT).

On the other hand, the antimicrobial material according to the present invention is microencapsulated and included in the antimicrobial coating solution composition, wherein the antimicrobial material is coated with a polymer on its outer wall surface as the core.

Here, the outer wall of the antimicrobial microcapsules may be any polymer that is commonly used in the art to form the outer wall of the microcapsules, but preferably made of melamine resin, urea resin and / or acrylic resin. It is good and melamine resin is recommended.

At this time, the antimicrobial microcapsules are microencapsulated by forming an outer wall, that is, a capsule layer on the outer circumferential surface of the antimicrobial material as a core, and the monomer for forming the outer wall polymerizes melamine resin, urea resin and / or acrylic resin. It is preferable to use monomers for the preparation, for example melamine monomers, acrylic monomers, urea monomers or mixtures thereof.

On the other hand, the method for producing a microcapsule containing an antimicrobial material according to the present invention may be used as long as it is a general microcapsulation (microcapsulation) method. As one example, in the present invention, it is recommended that the antimicrobial material is dispersed in an aqueous solution through an emulsification process and manufactured on the principle of polymerizing the polymer on the surface of the oil. The polymerization method is interfacial polymerization, in situ polymerization, and coacer. Since the reversal method can be used, it is preferable to manufacture using in situ polymerization.

Here, the method of microencapsulation has been widely used mainly in the pharmaceutical field, and recently has been applied to some food fields to protect the lactic acid bacteria in the stomach, to protect the material contained in the microcapsules from the external environment or It is used to control the release rate of the material.

In such a microencapsulation method, the core outer wall of the microcapsules can be classified into physical or chemical methods. As a physical method, a complex coacervation interface is a boundary between continuous and discontinuous phases. Precipitation of polymeric species at is used, for example, gelatin, gum arabic, vinylacetate-maleic anhydride copolymer, sodium alginate, polyacrylic acid and the like dissolved or dispersed in a continuous liquid phase at a controlled temperature and pH. Likewise, it reacts with an anion-charged colloid to coacetate or precipitate at the interface between the aqueous phase and the dispersed organic liquid phase. At this time, the wall or shell formed at the interface can be cured by physical or chemical treatment as disclosed in US Pat. No. 2,800,457.

In addition, the chemical method for forming the outer wall of the microcapsules is to disperse the urea and formaldehyde or urea-formaldehyde preagglomerate in a continuous liquid phase and then react to form an encapsulated shell around the dispersed phase containing the target material. Urea-formaldehyde aggregates are provided, which are disclosed in US Pat. Nos. 3,016,309 and 3,796,669.

Among the various microencapsulation methods as described above, the most widely used methods are interfacial polycondensation and in situ polymerization, and the in-situ polymerization method enables high yield and high concentration of encapsulation and thus is low in manufacturing cost. The advantage is that the encapsulation step can be easily controlled.

Thus, the in situ polymerization as an example of the method for producing the antimicrobial microcapsules according to the present invention will be described as follows.

First mixing 2 to 6 wt% of the dispersant per weight of the total reactant to 30 to 40 wt% of the solvent, followed by stirring for 20 to 40 minutes at a temperature of 60 to 90 ° C., followed by cooling;

30 to 40% by weight of the solvent is further mixed with the cooled mixture, followed by adding 15 to 25% by weight of the antimicrobial substance, followed by stirring at 1,500 to 1,900 rpm;

After adding 2 to 5% by weight of monomer and 3 to 6% by weight of formalin to form the outer wall of the microcapsules to the stirred mixture for 3 to 4 hours at a temperature of 50 to 80 ℃, preferably acid 1 to 3 Preparing a microcapsule slurry by polymerizing by stirring at 500 to 600 rpm while slowly adding weight%;

The microcapsule slurry prepared by the polymerization reaction is washed and then separated and dried to prepare an antimicrobial microcapsule.

Here, the solvent may be used as long as it is a solvent commonly used in the art for preparing antimicrobial microcapsules, but it is preferable to use water, specifically distilled water, and the amount of the total reactant is used. It is preferable to use 60 to 80% by weight relative to the weight.

In addition, the dispersant according to the present invention is not particularly limited, but preferably, an anionic water-soluble polymer, PSSA (Poly Styrene Sulfonic Acid) is used, and the amount of the dispersant is 2 to 6% by weight based on the total weight of the reactants. It is good.

The formalin according to the present invention is for crosslinking a monomer such as melamine monomer, acrylic monomer, urea monomer, etc. to form the outer wall of the microcapsules, and the amount of the formalin used is 3 to 6% by weight based on the total weight of the reactants. good.

The acid according to the present invention is a monomer for forming the outer wall of the microcapsules and formalin is added to the reaction to form a chain between the monomer and formalin by a condensation reaction, preferably polymerization to prepare the microcapsule slurry The reaction mixture is to maintain a pH suitable for polymerization at about 4, any acid that is commonly used in the art for preparing microcapsules may be used, but preferably acetic acid, about 0.2N concentration It is preferable to use an aqueous solution of hydrochloric acid or a mixture thereof, and the amount thereof is preferably used in an amount of 1 to 3% by weight based on the total weight of the reactants.

The antimicrobial microcapsules according to the present invention having such a configuration are mixed with other materials, specifically, a binder mixture to form an antimicrobial coating solution composition. The antimicrobial coating solution composition according to the present invention is antimicrobial microcapsules 15 to 25 by weight of the total coating solution. It is composed by mixing a weight percent, preferably about 20 weight percent and a binder mixture 75 to 85 weight percent, preferably about 80 weight percent.

Here, the binder mixture is to facilitate coating of the antimicrobial microcapsules on the object to be coated when the antimicrobial microcapsules are coated, but may be any conventional binder mixture used in the art for this purpose, but preferably Is 30 to 45% by weight of ethyl acrylate (preferably about 35% by weight); 0.5-1.5% by weight of N-Methylol Acryl Amide, preferably about 1% by weight; 0.1% to 1% by weight of ammonium persulfate, preferably about 0.5% by weight; 0.5 to 1.5% by weight, preferably about 1% by weight, of Ammonium Hydroxide; It is preferably composed of 1 to 2% by weight of methacrylic acid, preferably about 1.5% by weight and 50 to 70% by weight of solvent, preferably about 60% by weight.

Here, the solvent may be used as long as it is a solvent commonly used in the art used in the antimicrobial coating liquid composition, but preferably water, and specifically distilled water may be used.

On the other hand, the antimicrobial coating liquid composition according to the present invention having the above-described configuration can be used to be coated on a separate substrate, the "substrate" is to mean the target object is coated with the antimicrobial coating liquid composition according to the present invention, The antimicrobial coating liquid composition according to the present invention is coated on the surface of the substrate by dipping or spraying, so long as any bacteria and / or molds in contact with the substrate are removed.

As an example of such a substrate, the antimicrobial coating liquid composition according to the present invention may be coated and used on a filter filter, and the filter filter is used to be installed in a filter, preferably a deodorizing filter, for removing contaminants in the air. Any filter may be used as long as it is a conventional filter in the art.

Here, the deodorizing filter is a conventional filter in the art for removing contaminants such as odors contained in the air, and preferably includes a filter filter, more preferably activated carbon, preferably based on the plate-shaped activated carbon It is good that the filter filter is configured to be connected to the left and right (see Fig. 1).

Hereinafter, the present invention will be described in detail through examples. However, the following examples are only for illustrating the present invention in detail and are not intended to limit the scope of the present invention by these examples.

<Example 1>

Preparation of Antimicrobial Microcapsules.

20 g of PSSA (Poly Styrene Sulfonic Acid), an anionic water-soluble polymer, was added to 180 g of water as a dispersant and dissolved at 80 ° C. for stirring, followed by cooling for 30 minutes.

Then, 200 g of water was added to 200 g of the cooled solution, followed by stirring. Then, 250 g of 2-n-octyl-4-isothiazolin-3-one (OIT) [Daelim Chemical, South Korea] was added as an antimicrobial substance and then 1,700 rpm. After stirring at a rate of 15, melamine monomer 15g and formalin 18g to form the outer wall of the microcapsules were added, and acetic acid [Samjeon Chemical, Korea] was added while maintaining a stirring speed of 550rpm.

Then, the mixture was stirred at a reaction temperature of 60 ° C. for 3 to 4 hours to prepare a microcapsule in a slurry state.

Then, the slurry of the microcapsules was put into a vacuum filter and filtered using a filter paper (Glass Fiber Filters, pore size 0.30 μm [Whatman, USA]), washed with distilled water at least five times, separated, and dried. To prepare antimicrobial microcapsules.

The amount of the antimicrobial microcapsules prepared by this method was 240 g, the yield was about 84.8%, and the average particle size of the antimicrobial microcapsules was 0.8 to 2 μm. Here, the particle size distribution was measured using Scanning Electron Microscope (SEM, JEOL, JSM-6380LV, Japan).

<Example 2>

In the same manner as in Example 1, 2g of 0.2N HCl aqueous solution [Samjeon Chemical, Korea] was added to the mixture to be polymerized to maintain the pH of the mixture at 4.

As a result, the amount of the prepared antimicrobial microcapsules was 270 g, the yield was about 95.4%, and the average particle size of the antimicrobial microcapsules was 0.8 to 2 µm, similar to that of Example 1.

<Example 3>

Preparation of Antimicrobial Coating Liquid Composition.

20% by weight of the antimicrobial microcapsules prepared in Example 3, 18% by weight of ethyl acrylate [Samjeon Chemical, Korea], 1% by weight of N-methylol acrylamide [TCI, Japan], ammonium per 0.5% by weight of sulfate [Samjeon Chemical, Korea], 1% by weight of ammonium hydroxide [Aldrich, USA], 1.5% by weight of methacrylic acid [Samjeon Chemical, Korea] and 58% by weight of water contained antimicrobial microcapsules. An antimicrobial coating solution composition was prepared.

<Example 4>

Preparation of filter filter coated with antimicrobial coating solution.

The antimicrobial coating solution prepared according to Example 3 was dipped into a filter filter having a size of 20 × 20 cm [Filter Grade, Namyang Nonwovens Co., Ltd.] to coat the filter filter so that the concentration of the microcapsules was 5,000 ppm. Coated filtersheets were prepared.

<Example 5>

Preparation of Deodorization Filters.

As shown in FIG. 1, two filter filters manufactured according to Example 4 were connected to the left and right sides of activated carbon members manufactured by using a sheet of 20 × 20 cm sized activated carbon [GG Grade, Kuraray, Japan], respectively. Deodorizing filter was prepared.

<Example 6>

After diluting the antimicrobial coating solution prepared according to Example 3 to 10% by weight in distilled water to prepare a diluted antimicrobial coating solution composition using a sprayer of 20 × 20cm size so that the concentration of the final antimicrobial microcapsules 5,000ppm HEPA filter [Korea 3M, Korea] was sprayed to prepare a HEPA filter coated with antimicrobial microcapsules.

Comparative Example 1

15% by weight of solid DCOIT [Daelim Chemical, Korea], 15% by weight of ethyl alcohol [Samjeon Chemical, Korea], 13% by weight of ethyl acrylate [Samjeon Chemical, Korea] -Methylol acrylamide [TCI, Japan] 0.5% by weight, Ammonium persulfate [Samjeon Chemical, Korea] 1% by weight, Ammonium hydroxide [Aldrich, USA] 1.5% by weight, Methacrylic acid [Samjeon Chemical, Korea] 1 An antimicrobial coating solution composition was prepared by mixing the wt%, 1 wt% dispersant [Dispers 740W, TEGO, Germany] and 52 wt% water.

Then, using the antimicrobial coating solution composition was carried out sequentially as in Example 4 and Example 5 to prepare a deodorizing filter.

Comparative Example 2

The same procedure as in Comparative Example 1 was carried out, except that the liquid 2-n-octyl-4-isothiazolin-3-one (OIT) instead of 15% by weight of DCOIT (Daelim Chemical, Korea), which is a solid form, was used. [Daelim Chemical, Korea] 12% by weight of propylene glycol [Samjeon Chemical, Korea] was used instead of 18% by weight and 15% by weight of ethyl alcohol [Samjeon Chemical, Korea].

<Experiment>

Antimicrobial test

The antimicrobial test was carried out on the deodorizing filter of Example 5, Comparative Example 1 and Comparative Example 2 according to ATCC 100, inoculated with the inoculated microorganisms in the antimicrobial processed product and the control piece after measuring the number of viable cells Antimicrobial processed products and control pieces were compared.

Here, the test strain is Staphylococcus Aureus ) , and the antimicrobial evaluation method is shown in Equation 1 below, and the results are shown in Table 1 and FIGS. 2 to 4.

In Figures 2 to 4 (a) is a control specimen, (b) is a test specimen.

Percent reduction in bacterium = (B-C) / B × 100

here,

B is the viable count after 18 hours of the raw test piece,

C is the viable cell count after 24 hours of the antimicrobial processing test piece.

Antifungal ( Fungus ) exam

The antifungal test was conducted on the deodorizing filters of Example 5, Comparative Example 1 and Comparative Example 2 according to ISO846 Method B (fungal bacteriostatic effect test), by adding glucose to the spore suspension of five test molds. After the preparation, the suspension was uniformly sprayed on the sample and the plate medium, and then cultured for 4 weeks at 25 ° C temperature and 95% or higher humidity condition, the fungus growth test was performed to check the presence of antifungal activity.

Here, the test strain is Aspergillus niger ATCC 6275, Penicillium pinophilum ATCC 36839, Paecilomyces variotii ATCC 18502, Trichoderma virens ATCC 9645, Chaetomium globosum ATCC 6205, and the antimicrobial evaluation method is shown in Equation 1 below and the results are shown in Table 2 and FIGS.

In Figures 5 to 7 (a) is a sample immediately after the deodorization filter production, (b) is a sample 1 month after the deodorization filter production.

In Table 2, the evaluation method for each grade of test results is as follows.

Grade 0: Mold growth cannot be confirmed by naked eye or microscope, and if the development zone is recognized around the sample, the width is described in mm.

Grade 1: Mold growth is not visible to the naked eye, but microscopic.

Grade 2: The fungus grew slightly and did not exceed 25% of the sample area.

As shown in Table 2 and FIGS. 5 to 7, the deodorizing filter according to Example 5 exhibited excellent antifungal performance immediately after the deodorizing filter was manufactured as well as after 1 month of manufacture, but the thiazoline of Comparative Example 1 The deodorizing filter in the case of applying DCOIT, a solid antifungal agent of the system, did not satisfy the antifungal performance test according to ISO 846 Method B even immediately after preparation.

In addition, the deodorizing filter in which the liquid anti-fungal agent OIT of Comparative Example 2 was dispersed in a water-soluble acrylic binder also exhibited antifungal performance immediately after preparation of the deodorizing filter, but did not maintain antifungal performance after one month after manufacture. Appeared.

As described above, those skilled in the art will understand that the present invention can be implemented in other specific forms without changing the technical spirit or essential features. Therefore, the exemplary embodiments described above are to be understood as illustrative in all respects and not as restrictive. The scope of the present invention should be construed that all changes or modifications derived from the meaning and scope of the appended claims and their equivalents, rather than the detailed description, are included in the scope of the present invention.

The antimicrobial coating liquid composition comprising the antimicrobial microcapsules according to the present invention has the effect of continuously releasing antimicrobial substances from the microcapsules for a long time to maintain antibacterial and / or antifungal properties.

Claims (11)

An antimicrobial coating solution composition comprising 15 to 25% by weight of the antimicrobial microcapsules and 75 to 85% by weight of the binder mixture relative to the total coating weight. The method of claim 1, The binder mixture is 30 to 45 wt% ethyl acrylate, 0.5 to 1.5 wt% N-methylol acrylamide, 0.1 to 1 wt% ammonium persulfate, 0.5 to 1.5 wt% ammonium hydroxide, 1-2 to methacrylic acid An antimicrobial coating liquid composition comprising 50% by weight and 50% by weight of a solvent. The method of claim 1, The antimicrobial coating liquid composition characterized in that the antimicrobial microcapsules are formed by coating a melamine resin, urea resin, acrylic resin or a mixture thereof on the outer wall surface of the core made of an antimicrobial material. The method of claim 3, wherein The antimicrobial coating liquid composition, characterized in that the antimicrobial substance is 2-n-octyl-4-isothiazolin-3-one. Mixing 2 to 6 wt% of the dispersant per 30 wt% of the total reactant into 30 to 40 wt% of the solvent, followed by stirring for 20 to 40 minutes at a temperature of 60 to 90 ° C., followed by cooling; 30 to 40% by weight of the solvent is further mixed with the cooled mixture, followed by adding 15 to 25% by weight of the antimicrobial substance, followed by stirring at 1,500 to 1,900 rpm; 2 to 5% by weight of monomer and 3 to 6% by weight of formalin were added to the stirred mixture to form the outer wall of the microcapsules, followed by polymerization at 500 to 600 rpm for 3 to 4 hours at a temperature of 50 to 80 ° C. To prepare a microcapsule slurry; And 15 to 25% by weight of the antimicrobial microcapsules relative to the total weight of the coating liquid, and a method for producing an antimicrobial coating liquid composition comprising mixing 75 to 85% by weight of the binder mixture relative to the total weight of the coating liquid. The method of claim 5, The binder mixture is 30 to 45 wt% ethyl acrylate, 0.5 to 1.5 wt% N-methylol acrylamide, 0.1 to 1 wt% ammonium persulfate, 0.5 to 1.5 wt% ammonium hydroxide, 1-2 to methacrylic acid Method for producing an antimicrobial coating liquid composition comprising a weight percent and 50 to 70% by weight solvent. The method of claim 5, To prepare the microcapsule slurry further comprises 1 to 3% by weight of about 0.2N aqueous hydrochloric acid solution, acetic acid or a mixture thereof in order to maintain a pH suitable for polymerization in the mixture to the polymerization to 4 Method for producing an antimicrobial coating solution. The method of claim 5, The monomer for forming the outer wall of the microcapsules is a method for producing an antimicrobial coating liquid, characterized in that the melamine monomer, urea monomer, acrylic monomer or a mixture thereof. A filter coated with the antimicrobial coating liquid composition according to any one of claims 1 to 4. A deodorizing filter comprising a filter filter and activated carbon coated with the antimicrobial coating liquid composition according to claim 9. The method of claim 10, Deodorizing filter, characterized in that the filter filter is installed on the left / right of the deodorizing filter around the activated carbon.

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