JP7336157B2 - Antimicrobial composition and method for producing the same - Google Patents

Description

TECHNICAL FIELD The present invention relates to the technical field of antimicrobial compositions, and more particularly to an antimicrobial composition containing a photocatalyst and a method for producing the same.

With the improvement of people's living standards, the demand for cleanliness in the living environment is increasing day by day, which is driving the development of antimicrobial materials. However, conventional antimicrobial compositions usually contain additives such as antimicrobial chemicals, organic solvents and artificial flavors that can be harmful to the health of the body. Also, to enhance their effectiveness in inhibiting microbial growth, many conventional antimicrobial compositions are designed to be acidic or alkaline, causing damage to objects made from certain materials. This prevents users from applying or spraying conventional antimicrobial compositions onto various objects at will. For this reason, the new method can effectively suppress the growth of microorganisms, does not harm the health of the body, and can be sprayed on various objects without causing damage to the objects. There is a need to develop antimicrobial compositions.

For this reason, the new method can effectively suppress the growth of microorganisms, does not harm the health of the body, and can be sprayed on various objects without causing damage to the objects. There is a need to develop antimicrobial compositions.

In order to solve the aforementioned problems, the present invention provides a solution comprising: a plurality of photocatalyst particles; an aqueous layer of cypress distillate containing one or more kinds of aromatic compounds bound to the photocatalyst particles; Or, it contains a plurality of kinds of metal particles and a solvent, wherein the solvent is water, the photocatalyst particles are titanium oxide crystals, the metal particles are silver particles, and the water layer of the cypress distillate is 1,4-cineol, 1,8-cineol, fencon, fenchol, linalool, camphor, 1-terpineol, α-terpineol, α-dihydroterpineol, γ-terpineol, terpinen-4-ol, endo-borneol, m- Contains one or more aromatic compounds consisting of any one of isopropylphenol, citronellol and myrtanol.

In one embodiment, the content of the photocatalyst particles in the antimicrobial composition may be 1-10% by weight .

In one embodiment, the concentration of the metal particles in the antimicrobial composition may be 100-1000 ppm .

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 particle size of 1-5 nm.

The present invention further provides a method for producing an antimicrobial composition, comprising adding an aqueous layer of cypress distillate containing an aromatic compound, a photocatalyst precursor, and a metal ion compound into water to form a mixture; adding a solution to the mixed liquid to completely dissolve the aqueous layer of the cypress distillate containing the aromatic compound, the photocatalyst precursor, and the metal ion compound to make the mixed liquid a clear solution; and adding an alkaline solution to the clear solution, wherein the reducing agent reduces one or more metal ions of a metal ion compound to one or more metal particles, and the alkaline solution is a photocatalyst precursor. to form a photocatalytic intermediate, and wherein said metal particles and said aromatic compound are bound to said photocatalytic intermediate, and said photocatalytic intermediate and water deposited under said transparent solution. removing a viscous solution; removing charged ions derived from the acidic solution and the alkaline solution in the viscous solution to bring the pH value of the viscous solution to 6-8; Water is added to the viscous solution and stirred at 70-85° C. and 50-150 rpm until the photocatalyst intermediate product crystallizes to form photocatalyst particles, and contains 1-10% by weight of photocatalyst particles. forming a composition, wherein the photocatalytic precursor is titanium acetylacetone, the photocatalytic intermediate is titanium oxide, the photocatalytic particles are titanium oxide crystals, and the metal ion compound is silver nitrate. and the metal particles are silver particles, and the aqueous layer of the cypress distillate contains 1,4-cineol, 1,8-cineol, fenchone, fenchol, linalool, camphor, 1-terpineol, α-terpineol, One or more aromatic compounds consisting of any one of α-dihydroterpineol, γ-terpineol, terpinen-4-ol, endo-borneol, m-isopropylphenol, citronellol and myrtanol.

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

In one embodiment, prior to adding the photocatalyst precursor, the metal ion compound and the fragrance compound into water to form a mixture, the method for making the antimicrobial composition comprises extracting the fragrance compound from a plant. further includes

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. Said antimicrobial active ingredient can effectively inhibit the growth of microorganisms. In addition, the photocatalyst particles, metal particles, plant-extracted aromatic compounds and water itself and their combinations are all harmless to the body's health. Also, the pH of the antimicrobial composition is between 6 and 8, so that it does not cause damage to articles made of any material, and the user can apply the antimicrobial composition in various ways at will. It can be sprayed on anything.

FIG. 1 shows an antimicrobial composition of an embodiment of the invention.

The present invention provides an antimicrobial composition 100 comprising a plurality of photocatalytic particles 11, one or more metal particles 13, one or more aromatic compounds 15, and a solvent 20 (see Figure 1). . The metal particles 13 are bound to the photocatalyst particles 11 under the action of van der Waals forces. The aromatic compound 15 is bound to the photocatalytic particles 11 through its functional groups. The solvent 20 is water. The photocatalyst particles 11 combined with the metal particles 13 and the aromatic compound 15 are evenly 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 particles 11 may be ellipsoidal with a major axis of 15 to 20 nm and a minor axis of 6 to 10 nm. The surface area of the ellipsoidal photocatalyst particles 11 is larger than that of the spherical photocatalyst particles, so that they have stronger oxidizing power. The photocatalyst particles include 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, One or a plurality of photocatalyst particles made of any one of cobalt oxide, rhodium oxide, nickel oxide, rhenium oxide and zirconium oxide may be included, but not limited thereto. The material of the photocatalyst particles 11, after forming nanoparticles, converts oxygen or water into hydroxyl radicals (OH-) and superoxide anions when excited by light (visible light or ultraviolet light). Any semiconductor material can be used as long as it can be oxidized or reduced to radicals such as O2-). These radicals have strong oxidizing power and can destroy the structure of microorganisms such as bacteria and fungi. In other words, the photocatalytic particles 11 have antimicrobial effects such as antibacterial and antifungal effects. Moreover, the photocatalyst particles 11 have high chemical stability and do not emit harmful substances. In a specific embodiment, the photocatalyst particles 11 are anatase crystals of titanium oxide, 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 particle size of 1-5 nm. The metal particles may include one or more metal particles made of any one of silver, copper and platinum. The metal particles 13 may include one or a plurality of metal particles made of any one of silver, copper and platinum, but are not limited thereto. The material of the metal particles 13 may be any material capable of releasing metal ions having an antimicrobial effect. The metal ions can destroy microorganisms such as bacteria and fungi by interfering with cell wall synthesis, disrupting cell membranes, suppressing protein synthesis, and/or interfering with nucleic acid synthesis. In other words, the metal particles 13 have antimicrobial effects such as antibacterial and antifungal effects. Moreover, the metal particles 13 have high chemical stability and high safety.

In one embodiment, the aromatic compound 15 is extracted from a plant such as camphor, but is not limited to this. Said fragrance compound 15 may comprise a compound with antibacterial and/or antifungal effect. The aromatic compound 15 imparts a pleasing scent to the overall antimicrobial composition 100 . The aromatic compound 15 includes the following compounds: 1,4-cineole, 1,8-cineole, fenchone, fenchol, linalool ), camphor, 1-terpineol, α-terpineol, α-dihydro-terpineol, γ-terpineol, terpinene-4- may include one or more of terpinen-4-ol, endo-borneol, m-isopropylphenol, citronellol and myrtanol.

The present invention further provides a method of making the antimicrobial composition 100, comprising (1) adding the photocatalyst precursor, the metal ion compound and the aromatic compound 15 into water to form a mixture; completely dissolving the photocatalyst precursor, the metal ion compound and the aromatic compound 15 in addition to the mixed solution to make the mixed solution a clear solution; (3) adding a reducing agent and an alkaline solution to the clear solution; adding, wherein the reducing agent reduces one or more metal ions of a metal ion compound to one or more metal particles 13, and the alkaline solution forms a photocatalytic intermediate to a photocatalyst precursor. and the metal particles 13 and the aromatic compound 15 are bonded to the photocatalytic intermediates; (4) a viscous liquid containing the photocatalytic intermediates and water deposited under the transparent solution; (5) removing charged ions derived from the acidic solution and the alkaline solution in the viscous solution to bring the pH value of the viscous solution to 6-8; , (6) add water to the viscous solution and stir at 70-85°C and 50-150 rpm until the photocatalyst intermediate product crystallizes to form photocatalyst particles 11; and forming an antimicrobial composition 100 containing 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 may be vitamin C. The alkaline solution may be aqueous ammonia.

In one embodiment, prior to adding the photocatalyst precursor, the metal ion compound and the fragrance compound into water to form a mixture, the method for making the antimicrobial composition comprises extracting the fragrance compound from a plant. further includes

In the antimicrobial composition 100 provided by the present invention, the antimicrobial active ingredient is the photocatalyst particles 11 combined with the metal particles 13 and the aromatic compound 15, and the solvent 20 is water. Said antimicrobial active ingredient can effectively inhibit the growth of microorganisms. In addition, the photocatalyst particles 11, the metal particles 13, the plant-derived aromatic compound 15 and the solvent 20 themselves and their combinations are all harmless to physical health, and the antimicrobial composition 100 is good for physical health. Contains no additives such as antimicrobial chemicals, organic solvents and artificial flavors that may harm human health. Also, the pH of the antimicrobial composition 100 is between 6 and 8, so that it does not cause damage to articles made of any material, and the user can apply the antimicrobial composition 100 to various objects at will. can be sprayed on

In order to verify the excellent function of the antimicrobial composition 100 of the present invention in suppressing the growth of microorganisms, an antibacterial experiment and an antifungal experiment will be carried out using specific examples below.
[Preparation of Specific Examples]

Step 1: Extract aromatic compounds from Hinoki. Specifically, cypress is distilled by alternately using water distillation and steam distillation to obtain cypress distillate. The electrical conductivity of water used for distillation is approximately 20 μs/cm. The cypress distillate contains an oil layer and a water layer. The aqueous layer in the cypress distillate is taken out for subsequent steps. The water layer in the cypress distillate contains the following hydrophilic aromatic compounds: 1,4-cineol, 1,8-cineol, fencon, fenchol, linalool, camphor, 1-terpineol, α-terpineol, α- Including dihydroterpineol, gamma-terpineol, terpinen-4-ol, endo-borneol, m-isopropylphenol, citronellol and myrtanol. Step 1 may be omitted and subsequent steps may be performed instead using commercially available hydrophilic aromatic compounds extracted from Hinoki cypress.

Step 2: 145 g of titanium acetylacetonate, 2.5 g of silver nitrate and 1 kg of aqueous layer of cypress distillate and 2 kg of water are added to the reactor to form a mixture.

Step 3: Continue to add 1 M hydrogen chloride into the reaction vessel at a rate of about 10 cc/min to maintain the pH value of the mixture at 1-3, while rotating at a speed of 300-500 rpm to completely remove titanium acetylacetonate and silver nitrate. until it dissolves, thereby turning the mixture into a clear solution.

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

Step 5: Continue to add 15M ammonia water into the reactor at a rate of about 10cc/min to maintain the pH value of the clear solution at 9-10, while rotating at 300-500rpm to turn acetylacetone titanium into white titanium oxide. and the hydrophilic aromatic compound extracted from the cypress and the silver particles bind to the titanium oxide. Specifically, the silver particles bond with titanium atoms in titanium oxide by the action of van der Waals force. The aromatic compound binds to titanium oxide via its functional groups. Depending on the amount and time of addition of aqueous ammonia, the reduction of silver ions can be stopped, thereby controlling the size of the silver particles.

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

Step 7: ultrasonically vibrate the viscous solution for 60 minutes to evenly disperse the silver particles and the aromatic compound-bound titanium oxide in water, thereby turning the viscous solution into a homogenous solution; . This step may be omitted.

Step 8: remove chlorine ions (Cl-) derived from hydrogen chloride and ammonium ions (NH4+) derived from ammonia water in the uniform phase solution with a nuclear grade exchange resin, and adjust the pH value of the viscous solution to Make it 6-8.

Step 9: Filter out the nuclear grade resin in the homogenous solution with a filter plate. Specifically, the cavity dimensions of the filter plate are greater than the dimensions of the titanium oxide to which the silver particles and aroma compounds are bound and less than the dimensions of the nuclear grade resin. Upon filtering the phase homogenous solution through the filter plate, the nuclear grade resin remains on the filter plate, and the silver particles and titanium oxide to which the aromatic compound is bound and water pass through the filter plate. A homogeneous phase solution with a pH value of 6-8 is obtained.

Step 10: Add the homogeneous phase solution with a pH value of 6 to 8 into a stirring tank, add 20 μs/cm pure water until the total weight of the homogeneous phase solution reaches 10 kg, and pressurize at 70 to 85 ° C. , at a rotation speed of 50 to 150 rpm, stirring until titanium oxide crystallizes to form photocatalyst particles, adding about 1% by weight of photocatalyst particles (titanium oxide crystals), about 100 ppm of silver particles to the homogeneous phase solution, An antimicrobial composition is formed containing a hydrophilic aromatic compound of cypress and water. The pH value of said antimicrobial composition is 7.5. The photocatalyst particles (titanium oxide crystals) are ellipsoids having a major axis of 16-18 nm and a minor axis of 8-10 nm. The silver particles are spherical with a particle size of 1-2 nm. The silver particles bond with titanium atoms in the photocatalyst particles (titanium oxide crystals) by the action of van der Waals force. The aromatic compounds are bound to the photocatalyst particles via their functional groups.
[Antibacterial experiment]

The antimicrobial compositions of the foregoing specific examples were sent to SGS Taiwan Limited to be tested in <51> Antimicrobial Effectiveness Testing of Pharmacopeia Microbiological Tests in the United States. did. See Table 1 for test results.

A sterilization rate R<1% indicates no clear antibacterial effect. The sterilization rates R for Staphylococcus aureus, Escherichia coli and Klebsiella pneumoniae of the antimicrobial compositions of the foregoing specific examples are all above 99.9%. As can be seen, the antimicrobial compositions of the foregoing specific examples exhibit excellent antibacterial efficacy against both Gram-positive bacteria (Staphylococcus aureus) and Gram-negative bacteria (E. coli and Klebsiella pneumoniae). have.
[Antifungal experiment]

The antimicrobial compositions of the foregoing specific examples were sent to Taiwan Testing Technology Co., Ltd. and tested by <51> Antimicrobial Effectiveness Testing of Pharmacopeia Microbiological Tests, USA. The test results are as shown in Table 2.

A sterilization rate R<1% indicates no clear antifungal effect. The sterilization rates R for Candida albicans and Aspergillus brasilienis of the antimicrobial compositions of the above specific examples are all above 99.9%. As can be seen, the antimicrobial compositions of the foregoing specific examples all have excellent antifungal efficacy against various forms of fungi.

The foregoing are merely examples of the present invention and are not intended to limit the scope of the claims of the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the principles of the present invention should all be included in the scope of the claims of the present invention.

11 photocatalyst particles 13 metal particles 15 aromatic compound 20 solvent 100 antimicrobial composition

Claims (7)

a plurality of photocatalyst particles;
an aqueous layer of cypress distillate containing one or more aromatic compounds bound to the photocatalyst particles;
one or more metal particles bonded to the photocatalyst particles;
a solvent and
the solvent is water;
The photocatalyst particles are titanium oxide crystals, the metal particles are silver particles,
The aqueous layer of the cypress distillate includes 1,4-cineol, 1,8-cineol, fencon, fenchol, linalool, camphor, 1-terpineol, α-terpineol, α-dihydroterpineol, γ-terpineol, and terpinene-4. - an antimicrobial composition comprising one or more aromatic compounds consisting of any one of ol, endo-borneol, m-isopropylphenol, citronellol and myrtanol. 2. The antimicrobial composition according to claim 1, wherein the content of said photocatalyst particles in said antimicrobial composition is 1 to 10% by weight. The antimicrobial composition according to claim 1, wherein the concentration of said metal particles in said antimicrobial composition is from 100 to 1000 ppm. 2. The antimicrobial composition according to claim 1, wherein 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 particle size of 1-5 nm. adding an aqueous layer of cypress distillate containing an aromatic compound, a photocatalyst precursor, and a metal ion compound into water to form a mixture;
adding an acidic solution to the mixed liquid to completely dissolve the aqueous layer of the cypress distillate containing the aromatic compound, the photocatalyst precursor, and the metal ion compound to make the mixed liquid a clear solution;
adding a reducing agent and an alkaline solution to the clear solution, wherein the reducing agent reduces one or more metal ions of a metal ion compound to one or more metal particles, and the alkaline solution is a photocatalyst; causing a precursor to form a photocatalytic intermediate, and wherein the metal particles and the aromatic compound are bound to the photocatalytic intermediate;
removing a viscous solution containing the photocatalyst intermediate and water deposited under the transparent solution;
removing charged ions derived from the acidic solution and the alkaline solution in the viscous solution to bring the pH value of the viscous solution to 6 to 8;
Water is added to the viscous solution and stirred at 70-85° C. and 50-150 rpm until the photocatalyst intermediate product crystallizes to form photocatalyst particles, and contains 1-10% by weight of photocatalyst particles. forming a composition;
including
The photocatalyst precursor is titanium acetylacetone, 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,
The aqueous layer of the cypress distillate includes 1,4-cineol, 1,8-cineol, fencon, fenchol, linalool, camphor, 1-terpineol, α-terpineol, α-dihydroterpineol, γ-terpineol, and terpinene-4. - A process for the preparation of an antimicrobial composition comprising one or more aromatic compounds consisting of any one of ol, endo-borneol, m-isopropylphenol, citronellol and myrtanol. 6. The method for producing an antimicrobial composition according to claim 5 , wherein said acidic solution is hydrogen chloride, said reducing agent is vitamin C, and said alkaline solution is ammonia water. 6. The preparation of an antimicrobial composition according to claim 5 , further comprising extracting the aromatic compound from a plant before adding the photocatalyst precursor, the metal ion compound and the aromatic compound into water to form a mixture. Method.

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