TW202243739A - Antimicrobial composition and manufacturing method thereof - Google Patents

Abstract

The present invention provides an antimicrobial composition and a manufacturing method thereof. The antimicrobial composition includes a plurality of photocatalyst particles, one or more metal particles, one or more aromatic compounds, and a solvent. The metal particles and the aromatic compounds are combined to the photocatalyst particles. The solvent is water. The antimicrobial composition can effectively inhibit growth of microorganisms without harming human health, and can be sprayed on various objects without causing damage to the objects.

Description

Antimicrobial composition and method for its manufacture

The invention relates to the technical field of antimicrobial compositions, in particular to an antimicrobial composition containing a photocatalyst and a manufacturing method thereof.

With the improvement of people's living standards, the requirements for the cleanliness of the living environment are also increasing day by day, thus driving the development of anti-microbial materials. However, existing antimicrobial compositions generally contain chemical antimicrobial agents, organic solvents, and additives such as artificial flavors that may be harmful to human health. In addition, in order to strengthen the effect of inhibiting the growth of microorganisms, the existing antimicrobial compositions are mostly designed to be acidic or alkaline, which will cause damage to articles made of certain materials, so users cannot arbitrarily combine the existing antimicrobial compositions Coated or sprayed on various items. Therefore, there is a need to develop a novel antimicrobial composition, which can effectively inhibit the growth of microorganisms without endangering human health, and can be sprayed on various items without causing damage to the items.

In order to solve the aforementioned problems, the present invention provides an antimicrobial composition comprising a plurality of photocatalyst particles, one or more metal particles, one or more aromatic compounds and a solvent. The metal particle and the aromatic compound are combined on the photocatalyst particle. The solvent is water.

In one embodiment, the content of the photocatalyst particles in the antimicrobial composition may be 1-10% by weight. The photocatalyst particles may comprise one or more photocatalyst particles made of any of the following: titanium oxide, tin oxide, tungsten oxide, iron oxide, zinc oxide, chromium oxide, molybdenum oxide, ruthenium oxide, germanium oxide, lead oxide, oxide Cadmium, vanadium oxide, niobium oxide, tantalum oxide, manganese oxide, cobalt oxide, rhodium oxide, nickel oxide, rhenium oxide, and zirconium oxide.

In one embodiment, the concentration of the metal particles in the antimicrobial composition may be 100-1000 ppm. The metal particles may comprise one or more metal particles made from any of the following: silver, copper, and platinum.

In one embodiment, the photocatalyst particles are ellipsoids with a major axis of 15-20 nm and a minor axis of 6-10 nm, and the metal particles are spherical with a diameter of 1-5 nm.

The present invention also provides a method for producing an antimicrobial composition, which includes: adding the photocatalyst precursor, metal ion compound and aromatic compound into water to form a mixed solution; adding an acidic solution to the mixed solution to make the photocatalyst precursor, The metal ion compound and the aromatic compound are completely dissolved, so that the mixed solution becomes the transparent solution; a reducing agent and an alkaline solution are added to the transparent solution, wherein the reducing agent reduces one or more metal ions of the metal ion compound into one or more metal particles , the alkaline solution makes the photocatalyst precursor form a photocatalyst intermediate product, and the metal particles and the aromatic compound are combined on the photocatalyst intermediate product; take out the thick solution containing the photocatalyst intermediate product and water deposited on the lower layer of the transparent solution; removing charged ions from the acidic solution and the basic solution in the viscous solution, so that the pH of the viscous solution is 6-8; Stir at 50-150rpm until the photocatalyst intermediate product crystallizes to form photocatalyst particles, and then forms an antimicrobial composition containing 1-10% by weight of photocatalyst particles.

In one embodiment, the photocatalyst precursor is titanium acetylacetonate, the photocatalyst intermediate product is titanium oxide, the photocatalyst particles are titanium oxide crystals, the metal ion compound is silver nitrate, and the metal particles are silver particles.

In one embodiment, the acidic solution is hydrogen chloride, the reducing agent is vitamin C, and the alkaline solution is ammonia water.

In one embodiment, before the step of adding the photocatalyst precursor, the metal ion compound and the aromatic compound into water to form a mixed solution, the method for producing the antimicrobial composition further includes: extracting the aromatic compound from plants.

In the antimicrobial composition provided by the present invention, the antimicrobial active ingredient is photocatalyst particles combined with metal particles and aromatic compounds, and the solvent is water. The antimicrobial active ingredient can effectively inhibit the growth of microorganisms. Furthermore, the photocatalyst particles, metal particles, aromatic compounds extracted from plants, water itself and their combination will not harm human health. In addition, the pH of the antimicrobial composition is 6-8, so it will not cause damage to articles made of any material, so that users can freely spray the antimicrobial composition on various articles.

Please refer to FIG. 1 , the present invention provides an antimicrobial composition 100 comprising a plurality of photocatalyst particles 11 , one or more metal particles 13 , one or more aromatic compounds 14 and a solvent 20 . The metal particles 13 are combined with the photocatalyst particles 11 under the effect of van der Waals force. The aromatic compound 15 is combined with the photocatalyst particle 11 through its functional group. The solvent 20 is water. The photocatalyst particles 11 combined with the metal particles 13 and the aromatic compound 15 are uniformly dispersed in the antimicrobial composition 100 .

In one embodiment, the content of the photocatalyst particles in the antimicrobial composition may be 1-10% by weight. The photocatalyst particle 11 can be an ellipsoid with a major axis of 15-20 nm and a minor axis of 6-10 nm. Compared with spherical photocatalyst particles, the ellipsoidal photocatalyst particles 11 have a larger surface area, and thus have stronger oxidative power. The photocatalyst particles may comprise one or more photocatalyst particles made of any of the following: titanium oxide, tin oxide, tungsten oxide, iron oxide, zinc oxide, chromium oxide, molybdenum oxide, ruthenium oxide, germanium oxide, lead oxide, oxide Cadmium, vanadium oxide, niobium oxide, tantalum oxide, manganese oxide, cobalt oxide, rhodium oxide, nickel oxide, rhenium oxide, and zirconium oxide, but not limited thereto. The material of the photocatalyst particles 11 only needs to be able to oxidize or reduce oxygen or water into carboxyl radicals (hydrorxyl radical, OH ^- ) and superoxide anion (superoxide anion) when excited by light (visible light or ultraviolet light) after forming nanoparticles. Anion, O ₂ ^- ) and other free radical semiconductor materials will suffice. These free radicals have strong oxidizing power and can destroy the structure of microorganisms such as bacteria and mold. In other words, the photocatalyst particles 11 have antimicrobial effects such as antibacterial and antimildew. Furthermore, the photocatalyst particles 11 have high chemical stability and will not release harmful substances. In a specific embodiment, the photocatalyst particle 11 is anatase crystal of titanium oxide, which is also called "photosynthetic titanium".

In one embodiment, the concentration of the metal particles in the antimicrobial composition may be 100-1000 ppm. The metal particles 13 may be spherical with a diameter of 1-5 nm. The metal particles may comprise one or more metal particles made from any of the following: silver, copper, and platinum. The metal particles 13 may include one or more metal particles made of any of the following materials: silver, copper and platinum, but not limited thereto. The material of the metal particles 13 only needs to be a material capable of releasing metal ions having an antimicrobial effect. The metal ions can destroy microorganisms such as bacteria and molds by interfering with cell wall synthesis, damaging cell membranes, inhibiting protein synthesis and/or interfering with nucleic acid synthesis. In other words, the metal particles 13 have antimicrobial functions such as antibacterial and antimildew. Furthermore, the metal particles 13 have high chemical stability and high safety.

In one embodiment, the aroma compound 15 is extracted from plants, such as camphor tree, but not limited thereto. The aromatic compound 15 may include compounds with antibacterial and/or antifungal properties. The aroma compound 15 imparts a pleasant aroma to the antimicrobial composition 100 as a whole. The aromatic compound 15 may contain one or more of the following compounds: 1,4-cineole (1,4-cineole), 1,8-cineole (1,8-cineole), fenchone , fenchol (fenchol), linalool (linalool), camphor (camphor), 1-terpineol (1-terpineol), α-terpineol (α-terpineol), α-dihydroterpineol ( α-dihydro-terpineol), γ-terpineol (γ-terpineol), terpinen-4-ol (terpinen-4-ol), endo-borneol (endo-borneol), m-propofol (m -isopropylphenol), citronellol and myrtanol.

The present invention also provides a method for producing an antimicrobial composition 100, which includes: (1) adding the photocatalyst precursor, metal ion compound and aromatic compound 15 into water to form a mixed solution; (2) adding an acidic solution to the mixed solution , so that the photocatalyst precursor, metal ion compound and aromatic compound 15 are completely dissolved, so that the mixed solution becomes the transparent solution; (3) reducing agent and alkaline solution are added to the transparent solution, wherein the reducing agent makes the metal ion One or more metal ions of the compound are reduced to one or more metal ions 13, the alkaline solution causes the photocatalyst precursor to form a photocatalyst intermediate product, and the metal particles 13 and the aromatic compound 15 are combined on the photocatalyst intermediate product; (4) take out Deposit on the thick solution containing the photocatalyst intermediate product and water in the lower layer of the transparent solution; (5) remove the charged ions derived from the acidic solution and the alkaline solution in the thick solution, so that the thick solution The pH value is 6-8; and (6) adding water to the thick solution, and stirring at 50-150rpm at 70-85°C, until the photocatalyst intermediate product crystallizes to form photocatalyst particles 11, and then forms a photocatalyst particle containing 1-10% by weight Antimicrobial composition 100 of photocatalyst particles 11.

In one embodiment, the photocatalyst precursor is titanium acetylacetonate. The photocatalyst intermediate product is titanium oxide. The photocatalyst particles are titanium oxide crystals. The metal ion compound is silver nitrate. The metal particles are silver particles. The acidic solution may be hydrogen chloride. The reducing agent can be vitamin C. The alkaline solution can be ammonia water.

In one embodiment, before the step of adding the photocatalyst precursor, the metal ion compound and the aromatic compound into water to form a mixed solution, the method for producing the antimicrobial composition further includes: extracting the aromatic compound from plants.

In the antimicrobial composition 100 provided by the present invention, the antimicrobial active ingredient is the photocatalyst particle 11 combined with the metal particle 13 and the aromatic compound 15, and the solvent 20 is water. The antimicrobial active ingredient can effectively inhibit the growth of microorganisms. Furthermore, the photocatalyst particles 11, the metal particles 13, the aromatic compound 15 extracted from plants and the solvent 20 themselves and their combination will not harm human health; and the antimicrobial composition 100 does not contain chemical substances that may be harmful to human health. Antimicrobials, organic solvents, and additives such as artificial fragrances. In addition, the pH of the antimicrobial composition 100 is 6-8, so it will not cause damage to articles made of any material, so that users can freely spray the antimicrobial composition 100 on various articles.

In order to verify the excellent function of the antimicrobial composition 100 of the present invention in inhibiting the growth of microorganisms, the following specific examples were taken as examples to carry out antibacterial and antifungal experiments. Preparation of specific examples

Step 1: Extract aroma compounds from juniper wood. Specifically, water distillation and steam distillation are alternately used to distill cypress to obtain cypress distillate. The conductivity of the water used for distillation is about 20us/cm. The cypress distillate includes an oil layer and a water layer. The water layer in the cypress distillate was taken out for subsequent steps. The aqueous layer of this juniper wood distillate contains the following hydrophilic aromatic compounds: 1,4-cineol, 1,8-cineol, fenchone, fenchyl alcohol, linalool, camphorone, 1-terpineol , α-terpineol, α-dihydroterpineol, γ-terpineol, terpinen-4-ol, endo-borneol, m-propofol, citronellol and myrtenol. Step 1 can also be omitted, and a commercially available hydrophilic aromatic compound extracted from cypress is used instead to carry out the subsequent steps.

Step 2: Add 145g of titanium acetylacetonate, 2.5g of silver nitrate, 1Kg of the water layer of cypress distillate and 2Kg of water into the reaction tank to form a mixed solution.

Step 3: Add 1M hydrogen chloride to the reaction tank at a rate of about 10cc/min, so that the pH of the mixture is maintained at 1-3; at the same time, stir at a speed of 300-500rpm until titanium acetylacetonate and silver nitrate Dissolved completely so that the mixture became a clear solution.

Step 4: Add 5g of vitamin C into the reaction tank, and keep stirring at a speed of 300-500rpm to reduce the silver ions in the silver nitrate to silver particles.

Step 5: Continuously add 15M ammonia water to the reaction tank at a rate of about 10cc/min, so that the pH value of the transparent solution is maintained at 9-10; at the same time, continue to stir at a speed of 300-500rpm until titanium acetylacetonate is formed White titanium oxide, and the hydrophilic aromatic compound extracted from juniper wood and the silver particles are combined on the titanium oxide. Specifically, the silver particles are combined with the titanium atoms in the titanium oxide under the action of van der Waals force. The aromatic compound is bound to titanium oxide through its functional group. The reduction of silver ions can be stopped by the time and amount of ammonia water added, so as to control the size of silver particles.

Step 6: After standing still for 1-2 days, take out about 1-1.2Kg white thick solution deposited on the lower layer of the reaction tank. The white viscous solution contains titanium oxide combined with silver particles and aromatic compounds, and water.

Step 7: The viscous solution was oscillated by ultrasonic waves for 60 minutes, so that the titanium oxide combined with silver particles and aromatic compounds was uniformly dispersed in water, so that the viscous solution became a homogeneous solution. This step can also be omitted.

Step 8: Using a nuclear grade exchange resin to remove chloride ions (Cl ⁻ ) derived from hydrogen chloride and ammonium ions (NH4 ⁺ ) derived from ammonia water in the homogeneous solution, so that the pH of the thick solution is 6-8.

Step 9: Filter out the nuclear-grade resin in the homogeneous solution with a filter plate. Specifically, the pore size of the filter plate is larger than that of titanium oxide combined with silver particles and aromatic compounds, and smaller than that of nuclear grade resin. When the homogeneous solution is filtered by the filter plate, the nuclear grade resin will remain on the filter plate, and titanium oxide and water combined with silver particles and aromatic compounds will flow through the filter plate to obtain a pH value of 6-8 homogeneous solution.

Step 9: Add the homogeneous solution with a pH value of 6-8 into the stirring tank, and add 20 us/cm of pure water until the total weight of the homogeneous solution is 10 Kg; and at a normal pressure of 70-85°C Stir at a speed of 50-150 rpm until titanium oxide crystals form photocatalyst particles, so that the homogeneous solution forms photocatalyst particles (titanium oxide crystals) containing about 1% by weight, about 100 ppm silver particles, and the hydrophilicity of the aforementioned juniper wood. Antimicrobial composition of aromatic compounds and water. The pH of the antimicrobial composition was 7.5. The photocatalyst particle (titanium oxide crystal) is an ellipsoid with a long diameter of 16-18 nm and a short diameter of 8-10 nm. The silver particles are spherical with a particle diameter of 1-2 nm. The silver particle is combined with the titanium atom in the photocatalyst particle (titanium oxide crystal) under the action of van der Waals force. The aromatic compound is combined with the photocatalyst particle through its functional group. Antibacterial test

The antimicrobial composition of the above-mentioned specific examples was sent to SGS Taiwan Limited (SGS Taiwan Limited) for testing by <51> Antimicrobial Effectiveness Testing of Pharmacopeia Microbiological Tests in the United States. See Table 2 for test results. [Table 2] strain name ATCC number The amount of original inoculum (CFU/mL) Action time of antimicrobial composition (Min) The amount of bacteria after action (CFU/mL) Sterilization rate R (%) Staphylococcus aureus 6538 3.7×10 ⁵ 30 <1 >99.9 Escherichia coli 8739 4.2×10 ⁵ 30 <1 >99.9 Klebsiella pneumoniae 10231 2.5×10 ⁵ 30 <1 >99.9

When the sterilization rate R<1%, it means that there is no obvious antibacterial effect. The sterilization rate R of the antimicrobial composition of the foregoing specific examples for Staphylococcus aureus, Escherichia coli and Klebsiella pneumoniae is all greater than 99.9%. It can be seen that the antimicrobial composition of the aforementioned specific examples has excellent antibacterial effect on Gram-positive bacteria (Staphylococcus aureus) and Gram-negative bacteria (Escherichia coli and Klebsiella pneumoniae). . Antifungal test

The antimicrobial composition of the foregoing specific examples was sent to Taiwan Inspection Technology Co., Ltd. for testing by <51> Antimicrobial Effectiveness Testing of Pharmacopeia Microbiological Tests in the United States. For test results, please refer to Table 3, [Table 3] strain name ATCC number The amount of original inoculum (CFU/mL) Action time of antimicrobial composition (Min) The amount of bacteria after action (CFU/mL) Sterilization rate R (%) Candida albicans 10231 2.5×10 ⁵ 30 <1 >99.9 Aspergillus black yeast 16404 2.0×10 ⁵ 60 <1 >99.9

When the sterilization rate R<1%, it means that there is no obvious antifungal effect. The sterilization rate R of the antimicrobial composition of the foregoing specific examples for Candida albicans and Aspergillus brasilienis is greater than 99.9%. It can be seen that the antimicrobial composition of the foregoing specific examples has excellent antifungal effects on different types of fungi.

The above description is only an embodiment of the present invention, and is not intended to limit the patent scope of the present invention. Any modifications, equivalent replacements and improvements made within the principles of the present invention should be included in the patent scope of the present invention. within.

11: Photocatalyst particles 13: Metal particles 15: Aromatic compounds 20: Solvent 100: Antimicrobial Composition

[ Fig. 1 ] is a schematic diagram of an antimicrobial composition according to an example of the present invention.

11: Photocatalyst particles

13: Metal particles

15: Aromatic compounds

20: Solvent

100: Antimicrobial Composition

Claims (10)

An antimicrobial composition comprising: Multiple photocatalyst particles; One or more aromatic compounds are combined on the photocatalyst particles; one or more metal particles, combined on the photocatalyst particle; and A solvent, wherein the solvent is water. The antimicrobial composition as claimed in item 1, wherein the content of the photocatalyst particles in the antimicrobial composition is 1-10% by weight. Such as the antimicrobial composition of claim 1, wherein the photocatalyst particles comprise one or more photocatalyst particles made of any of the following: titanium oxide, tin oxide, tungsten oxide, iron oxide, zinc oxide, chromium oxide, molybdenum oxide, Ruthenium oxide, germanium oxide, lead oxide, cadmium oxide, vanadium oxide, niobium oxide, tantalum oxide, manganese oxide, cobalt oxide, rhodium oxide, nickel oxide, rhenium oxide, and zirconium oxide. The antimicrobial composition according to claim 1, wherein the concentration of the metal particles in the antimicrobial composition is 100-1000 ppm. The antimicrobial composition according to claim 1, wherein the metal particles comprise one or more metal particles made of any of the following: silver, copper and platinum. The antimicrobial composition as claimed in claim 1, wherein the photocatalyst particles are ellipsoids with a long diameter of 15-20 nm and a short diameter of 6-10 nm, and the metal particles are spherical with a diameter of 1-5 nm. A method for producing an antimicrobial composition, comprising: adding the photocatalyst precursor, metal ion compound and aromatic compound into water to form a mixed solution; Adding an acidic solution to the mixed solution to completely dissolve the photocatalyst precursor, metal ion compound and aromatic compound, so that the mixed solution becomes the transparent solution; Add a reducing agent and an alkaline solution to the transparent solution, wherein the reducing agent reduces one or more metal ions of the metal ion compound into one or more metal particles, the alkaline solution makes the photocatalyst precursor form a photocatalyst intermediate product, and the metal particle Combine with the aromatic compound on the photocatalyst intermediate product; Take out the viscous solution containing the photocatalyst intermediate product and water deposited on the lower layer of the transparent solution; removing charged ions from the acidic solution and the alkaline solution in the viscous solution, so that the pH of the viscous solution is 6-8; and Add water to the thick solution and stir at 50-150rpm at 70-85°C until the photocatalyst intermediate product crystallizes to form photocatalyst particles, thereby forming an antimicrobial composition containing 1-10% by weight of photocatalyst particles. Such as the manufacture method of the antimicrobial composition of claim 7, wherein the photocatalyst precursor is titanium acetylacetonate, the photocatalyst intermediate product is titanium oxide, the photocatalyst particles are titanium oxide crystals, the metal ion compound is silver nitrate, and the metal The particles are silver particles. The method for producing an antimicrobial composition as claimed in claim 8, wherein the acidic solution is hydrogen chloride, the reducing agent is vitamin C, and the alkaline solution is ammonia water. The manufacturing method of the antimicrobial composition according to claim 7, before the step of adding the photocatalyst precursor, the metal ion compound and the aromatic compound into water to form a mixed solution, further comprising: extracting the aromatic compound from plants.

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