CN108864880A - A kind of antimicrobial coating and its preparation process - Google Patents
A kind of antimicrobial coating and its preparation process Download PDFInfo
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- CN108864880A CN108864880A CN201810861109.2A CN201810861109A CN108864880A CN 108864880 A CN108864880 A CN 108864880A CN 201810861109 A CN201810861109 A CN 201810861109A CN 108864880 A CN108864880 A CN 108864880A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/14—Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
- C09D133/16—Homopolymers or copolymers of esters containing halogen atoms
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The present invention relates to a kind of antimicrobial coating and its preparation process, the antimicrobial coating includes the Fe of mass percentage %0.01-%0.053O4Adulterate TiO2Nanoparticle, it further include fluorine-containing lotion, epoxy resin latex, melamine, carbodiimides, talcum powder, sodium polymethacrylate, aqueous color paste, trimethyl hydroxyl amylalcohol isobutyrate, propylene glycol, the fatty acid ester compounded object of higher alcohols, titanium dioxide, polyoxyethylene alkylphenol base ether, 1,2 benzisothiazole-3-ketones, alkanolamine and water, the present invention is blended by the component, the Fe3O4Adulterate TiO2Nanoparticle is by Ti (SO4)2、Fe3O4, ammonium hydroxide, neopelex, nitric acid, hydrochloric acid and water be prepared by co-precipitation, relative to containing pure TiO2The antimicrobial coating of nanoparticle, the present invention have broader absorption spectrum, still have very strong antibacterial sterilizing activity under visible light, and need less nanoparticle in production process, significantly reduce cost.
Description
Technical field
The present invention relates to technical field of coatings, more particularly, to a kind of antimicrobial coating and its preparation process.
Background technique
Antimicrobial coating is a kind of coating technology developed rapidly in recent years, and antimicrobial coating is applied to medical space, energy
The propagation for significantly inhibiting pathogenic microorganism has very important meaning to public health, in actual application, photocatalysis half
Conductor nano material TiO2The most universal with ZnO, photocatalysis sterilization principle is photocatalytic semiconductor material under the irradiation of ultraviolet light
Expect that surface generates a large amount of hydroxyl radical free radical and oxygen radical, there is very strong and chemical activity, make microorganism that organic substance occur
Oxidation reaction, so that inhibition and killing effect are played to the microorganism contacted with film, since nanoparticle itself does not participate in instead
It answers, and the oxidative free radical on surface can be constantly regenerating under ultraviolet light, so, mixed with photocatalytic semiconductor nano material
Coating there is longer service life, and as most-often used TiO2There is excellent, cheap, abundance again
The characteristics of, thus TiO2Nano material is most widely used.
However photocatalytic substance is usually to have special optical wavelength absorption region, TiO2Nanoparticle has ultraviolet light
There are very strong absorption intensity and sterilizing activity, and absorb under visible light weak, activity is weak, therefore in some corners for loseing sunlight
In just at corner or spot as yet untouched by a clean-up campaign, in order to solve this problem, have more excellent properties sterilization coating needs be developed.
Summary of the invention
In view of prior art scenario, to solve the deficiencies in the prior art, the present invention provides one kind also to have under visible light
The sterilizing coating of strong sterilizing activity, and propose a kind of preparation process.
A kind of antimicrobial coating, the antimicrobial coating include Fe3O4Adulterate TiO2Nanoparticle, the antimicrobial coating further include
The component of following parts by weight, 20-40 parts of fluorine-containing lotion, 20-40 parts of epoxy resin latex, 0.1-1.5 parts of melamine,
0.1-1.5 parts of carbodiimides, 20-40 parts of talcum powder, 1-3 parts of sodium polymethacrylate, 8-55 parts of aqueous color paste, trimethyl hydroxyl
1-3 parts of amylalcohol isobutyrate, 0-2 parts of propylene glycol, fatty acid ester compounded object 0.5-1.0 parts of higher alcohols, 20-40 parts of titanium dioxide, gather
0.2-0.4 parts of ethylene oxide alkyl phenol ether through reaction, 1,2 0.4-0.6 parts of benzisothiazole-3-ketone, 0.5-0.7 parts of alkanolamine, water
40-60 parts.
Preferably, the antimicrobial coating further includes the component of following parts by weight, and 30 parts of fluorine-containing lotion, epoxy resin
30 parts of lotion, 0.8 part of melamine, 0.9 part of carbodiimides, 33 parts of talcum powder, 2 parts of sodium polymethacrylate, aqueous color paste
25 parts, 2 parts of isobutyrate of trimethyl hydroxyl amylalcohol, 1.2 parts of propylene glycol, 0.8 part of the fatty acid ester compounded object of higher alcohols, titanium dioxide 28
Part, 0.3 part of polyoxyethylene alkylphenol base ether, 1,2 0.5 part of benzisothiazole-3-ketone, 0.6 part of alkanolamine, 50 parts of water.
Preferably, the Fe3O4Adulterate TiO2Fe in nanoparticle3O4Mass percentage is 0.03-0.07%.
Preferably, Fe in the antimicrobial coating3O4Adulterate TiO2Nanoparticle mass percentage is 0.01-0.05%.
Preferably, the Fe3O4Adulterate TiO2Nanoparticle is by Ti (SO4)2、Fe3O4, ammonium hydroxide, neopelex,
Nitric acid, hydrochloric acid and water are prepared by co-precipitation.
A kind of preparation process of antimicrobial coating, includes the following steps：
(1) Fe is prepared3O4Adulterate TiO2Nanoparticle；
(2) by Fe3O4Adulterate TiO2Nanoparticle is dispersed in water, and moderate-speed mixer 10-30min is placed on microwave disperser
Fe is made in middle dispersion 10-30min3O4Adulterate TiO2Nanoparticle dispersion liquid；
(3) by water, Fe3O4Adulterate TiO2Nanoparticle dispersion liquid, titanium dioxide, 1,2 benzisothiazole-3-ketone polyoxy second
Allylic alkylation phenol ether through reaction is placed in moderate-speed mixer 20-40min in reaction vessel, and fluorine-containing propene yogurt is then added under stirring
Liquid, epoxy resin latex, melamine, carbodiimides, talcum powder, sodium polymethacrylate, aqueous color paste and alkanolamine,
Trimethyl hydroxyl amylalcohol isobutyrate, propylene glycol and higher alcohols fat is added after high-speed stirred 30-60min in the case where switching to moderate-speed mixer
Acid esters compound, moderate-speed mixer 10-30min；
(4) it by the mixture prepared through filter cleaning, then measures, pack, storage saves.
Preferably, the Fe3O4Adulterate TiO2The preparation of nanoparticle includes the following steps
(1) by Ti (SO4)2It is dispersed in water, high-speed stirred 10-20min, ammonium hydroxide is added and adjusts solution to acidity, continues to stir
20-40min is mixed, is filtered after standing 30-60min, dries to obtain solid after cleaning 3-5 times：
(2) solid that the step (1) obtains is dissolved with nitric acid solution, is filtered, collected filtrate, ten are added in filtrate
Dialkyl benzene sulfonic acids sodium adjusts soda acid to faintly acid with ammonium hydroxide；
(3) by Fe3O4It is dissolved in hydrochloric acid solution, the step (2) resulting solution is then added, adjust solution with ammonium hydroxide
To neutrality, moderate-speed mixer 60-120min then stands 30-60min, filters, and rinses, and repeats 3-5 times；
(4) by 450-550 DEG C of calcining 2-5h of the step (3) resulting solid, grinding obtains Fe after natural cooling3O4It mixes
Miscellaneous TiO2Nanoparticle.
Wherein, the nitric acid is 0.3-0.8mol/L.
Beneficial effect
1, the present invention contains Fe3O4Adulterate TiO2Nanoparticle, relative to pure TiO2Nanoparticle, Fe3O4Adulterate TiO2Nanometer
Particle has broader absorption spectrum, can absorb visible light and generate excitation, forms oxidisability, still has under visible light very strong
Antibacterial sterilizing activity, enable to the insufficient corner or spot as yet untouched by a clean-up campaign of ultraviolet light that can also have sufficiently strong sterilizing activity.
2, the present invention can reach identical bactericidal effect using less fungicide nanoparticle, save in process of production
Raw material is saved, cost is significantly reduced, increases economic and practical.
Specific embodiment
The present invention is described in further detail below by specific embodiment, but not limited to this, it is common in this field
Technical staff within the scope of knowledge, can also make a variety of changes, modify without departing from the purpose of the present invention,
Replacement and variant, the scope of the present invention is defined by the appended.
Embodiment 1：
A kind of antimicrobial coating, the antimicrobial coating include Fe3O4TiO2 nanoparticle is adulterated, the antimicrobial coating further includes
The component of following parts by weight, 20 parts of fluorine-containing lotion, 20 parts of epoxy resin latex, 0.1 part of melamine, carbodiimides
0.1 part, 20 parts of talcum powder, 1 part of sodium polymethacrylate, 8 parts of aqueous color paste, 1 part of isobutyrate of trimethyl hydroxyl amylalcohol, higher alcohols
0.5 part of fatty acid ester compounded object, 20 parts of titanium dioxide, 0.2 part of polyoxyethylene alkylphenol base ether, 1,2 benzisothiazole-3-ketone
0.4 part, 0.5 part of alkanolamine, 40 parts of water.
The Fe3O4Adulterate Fe in TiO2 nanoparticle3O4Mass percentage is 0.03%.
Fe in the antimicrobial coating3O4Adulterate TiO2Nanoparticle mass percentage is 0.01%.
The Fe3O4Adulterate TiO2Nanoparticle is by Ti (SO4)2、Fe3O4, ammonium hydroxide, neopelex, nitric acid, salt
Acid and water are prepared by co-precipitation.
A kind of preparation process of antimicrobial coating, includes the following steps：
(1) Fe is prepared3O4Adulterate TiO2Nanoparticle；
(2) by Fe3O4Adulterate TiO2Nanoparticle is dispersed in water, and moderate-speed mixer 10min, which is placed in microwave disperser, to be divided
Fe is made in scattered 10min3O4Adulterate TiO2Nanoparticle dispersion liquid；
(3) by water, Fe3O4Adulterate TiO2Nanoparticle dispersion liquid, titanium dioxide, 1,2 benzisothiazole-3-ketone polyoxy second
Allylic alkylation phenol ether through reaction is placed in moderate-speed mixer 20min in reaction vessel, and fluorine-containing lotion, ring are then added under stirring
Oxygen resin emulsion, melamine, carbodiimides, talcum powder, sodium polymethacrylate, aqueous color paste and alkanolamine, high speed
Trimethyl hydroxyl amylalcohol isobutyrate is added in the case where switching to moderate-speed mixer after stirring 30min, propylene glycol and high-carbon alcohol fatty acid ester are multiple
Close object, moderate-speed mixer 10min；
(4) it by the mixture prepared through filter cleaning, then measures, pack, storage saves.
The Fe3O4Adulterate TiO2The preparation of nanoparticle includes the following steps：
(1) by Ti (SO4)2It is dispersed in water, high-speed stirred 10min, ammonium hydroxide is added and adjusts solution to acidity, continues to stir
20min is filtered after standing 30min, dries to obtain solid after cleaning 3 times：
(2) solid that the step (1) obtains is dissolved with nitric acid solution, is filtered, collected filtrate, ten are added in filtrate
Dialkyl benzene sulfonic acids sodium adjusts soda acid to faintly acid with ammonium hydroxide；
(3) by Fe3O4It is dissolved in hydrochloric acid solution, the step (2) resulting solution is then added, adjust solution with ammonium hydroxide
To neutrality, moderate-speed mixer 60min then stands 30min, filters, and rinses, is repeated 3 times；
(4) by 450 DEG C of calcining 2h of the resulting solid of the step (3), grinding obtains Fe after natural cooling3O4Adulterate TiO2
Nanoparticle.
Wherein, the nitric acid is 0.3mol/L.
Embodiment 2：
A kind of antimicrobial coating, the antimicrobial coating include Fe3O4Adulterate TiO2Nanoparticle, the antimicrobial coating further include
The component of following parts by weight, 40 parts of fluorine-containing lotion, 40 parts of epoxy resin latex, 1.5 parts of melamine, carbodiimides
1.5 parts, 40 parts of talcum powder, 3 parts of sodium polymethacrylate, 55 parts of aqueous color paste, 3 parts of isobutyrate of trimethyl hydroxyl amylalcohol, the third two
2 parts of alcohol, 1.0 parts of the fatty acid ester compounded object of higher alcohols, 40 parts of titanium dioxide, 0.4 part of polyoxyethylene alkylphenol base ether, 1,2 benzisoxa
0.6 part of thiazoline -3- ketone, 0.7 part of alkanolamine, 60 parts of water.
The Fe3O4Adulterate TiO2Fe in nanoparticle3O4Mass percentage is 0.04%.
Fe in the antimicrobial coating3O4Adulterate TiO2Nanoparticle mass percentage is 0.02%.
The Fe3O4Adulterate TiO2Nanoparticle is by Ti (SO4)2、Fe3O4, ammonium hydroxide, neopelex, nitric acid, salt
Acid and water are prepared by co-precipitation.
A kind of preparation process of antimicrobial coating, includes the following steps：
(1) Fe is prepared3O4Adulterate TiO2Nanoparticle；
(2) by Fe3O4Adulterate TiO2Nanoparticle is dispersed in water, and moderate-speed mixer 20min, which is placed in microwave disperser, to be divided
Fe is made in scattered 10-30min3O4Adulterate TiO2Nanoparticle dispersion liquid；
(3) by water, Fe3O4Adulterate TiO2Nanoparticle dispersion liquid, titanium dioxide, 1,2 benzisothiazole-3-ketone polyoxy second
Allylic alkylation phenol ether through reaction is placed in moderate-speed mixer 30min in reaction vessel, and fluorine-containing lotion, ring are then added under stirring
Oxygen resin emulsion, melamine, carbodiimides, talcum powder, sodium polymethacrylate, aqueous color paste and alkanolamine, high speed
Trimethyl hydroxyl amylalcohol isobutyrate is added in the case where switching to moderate-speed mixer after stirring 30min, propylene glycol and high-carbon alcohol fatty acid ester are multiple
Close object, moderate-speed mixer 10min；
(4) it by the mixture prepared through filter cleaning, then measures, pack, storage saves.
The Fe3O4Adulterate TiO2The preparation of nanoparticle includes the following steps：
(1) by Ti (SO4)2It is dispersed in water, high-speed stirred 20min, ammonium hydroxide is added and adjusts solution to acidity, continues to stir
40min is filtered after standing 60min, dries to obtain solid after cleaning 3 times：
(2) solid that the step (1) obtains is dissolved with nitric acid solution, is filtered, collected filtrate, ten are added in filtrate
Dialkyl benzene sulfonic acids sodium adjusts soda acid to faintly acid with ammonium hydroxide；
(3) by Fe3O4It is dissolved in hydrochloric acid solution, the step (2) resulting solution is then added, adjust solution with ammonium hydroxide
To neutrality, moderate-speed mixer 120min then stands 60min, filters, and rinses, is repeated 5 times；
(4) by 550 DEG C of calcining 5h of the resulting solid of the step (3), grinding obtains Fe after natural cooling3O4Adulterate TiO2
Nanoparticle.
Wherein, the nitric acid is 0.8mol/L.
Embodiment 3：
A kind of antimicrobial coating, the antimicrobial coating include Fe3O4Adulterate TiO2Nanoparticle, the antimicrobial coating further include
The component of following parts by weight, 25 parts of fluorine-containing lotion, 28 parts of epoxy resin latex, 0.8 part of melamine, carbodiimides
0.8 part, 25 parts of talcum powder, 1.5 parts of sodium polymethacrylate, 12 parts of aqueous color paste, 2 parts of isobutyrate of trimethyl hydroxyl amylalcohol, third
0.5 part of glycol, 0.8 part of the fatty acid ester compounded object of higher alcohols, 26 parts of titanium dioxide, 0.25 part of polyoxyethylene alkylphenol base ether, 1,2 benzene
And 0.45 part of isothiazoline -3- ketone, 0.55 part of alkanolamine, 45 parts of water.
The Fe3O4Adulterate TiO2Fe in nanoparticle3O4Mass percentage is 0.05%.
Fe in the antimicrobial coating3O4Adulterate TiO2Nanoparticle mass percentage is 0.03%.
The Fe3O4Adulterate TiO2Nanoparticle is by Ti (SO4)2、Fe3O4, ammonium hydroxide, neopelex, nitric acid, salt
Acid and water are prepared by co-precipitation.
A kind of preparation process of antimicrobial coating, includes the following steps：
(1) Fe is prepared3O4Adulterate TiO2Nanoparticle；
(2) by Fe3O4Doping TiO2 nanoparticle is dispersed in water, and moderate-speed mixer 15min, which is placed in microwave disperser, to be divided
Fe is made in scattered 15min3O4Adulterate TiO2Nanoparticle dispersion liquid；
(3) by water, Fe3O4Adulterate TiO2Nanoparticle dispersion liquid, titanium dioxide, 1,2 benzisothiazole-3-ketone polyoxy second
Allylic alkylation phenol ether through reaction is placed in moderate-speed mixer 25min in reaction vessel, and fluorine-containing lotion, ring are then added under stirring
Oxygen resin emulsion, melamine, carbodiimides, talcum powder, sodium polymethacrylate, aqueous color paste and alkanolamine, high speed
Trimethyl hydroxyl amylalcohol isobutyrate is added in the case where switching to moderate-speed mixer after stirring 40min, propylene glycol and high-carbon alcohol fatty acid ester are multiple
Close object, moderate-speed mixer 15min；
(4) it by the mixture prepared through filter cleaning, then measures, pack, storage saves.
The Fe3O4Adulterate TiO2The preparation of nanoparticle includes the following steps：
(1) by Ti (SO4)2It is dispersed in water, high-speed stirred 15min, ammonium hydroxide is added and adjusts solution to acidity, continues to stir
25min is filtered after standing 35min, dries to obtain solid after cleaning 5 times：
(2) solid that the step (1) obtains is dissolved with nitric acid solution, is filtered, collected filtrate, ten are added in filtrate
Dialkyl benzene sulfonic acids sodium adjusts soda acid to faintly acid with ammonium hydroxide；
(3) by Fe3O4It is dissolved in hydrochloric acid solution, the step (2) resulting solution is then added, adjust solution with ammonium hydroxide
To neutrality, moderate-speed mixer 80min then stands 45min, filters, and rinses, is repeated 5 times；
(4) by 480 DEG C of calcining 3h of the resulting solid of the step (3), grinding obtains Fe after natural cooling3O4Adulterate TiO2
Nanoparticle.
Wherein, the nitric acid is 0.5mol/L.
Embodiment 4：
A kind of antimicrobial coating, the antimicrobial coating include Fe3O4Adulterate TiO2Nanoparticle, the antimicrobial coating further include
The component of following parts by weight, 35 parts of fluorine-containing lotion, 35 parts of epoxy resin latex, 1.2 parts of melamine, carbodiimides
1.2 parts, 35 parts of talcum powder, 2.5 parts of sodium polymethacrylate, 50 parts of aqueous color paste, 2.5 parts of isobutyrate of trimethyl hydroxyl amylalcohol,
1.5 parts of propylene glycol, 0.8 part of the fatty acid ester compounded object of higher alcohols, 35 parts of titanium dioxide, 0.33 part of polyoxyethylene alkylphenol base ether, 1,2
0.55 part of benzisothiazole-3-ketone, 0.6 part of alkanolamine, 55 parts of water.
The Fe3O4Adulterate TiO2Fe in nanoparticle3O4Mass percentage is 0.06%.
Fe in the antimicrobial coating3O4Adulterate TiO2Nanoparticle mass percentage is 0.04%.
The Fe3O4Adulterate TiO2Nanoparticle is by Ti (SO4)2、Fe3O4, ammonium hydroxide, neopelex, nitric acid, salt
Acid and water are prepared by co-precipitation.
A kind of preparation process of antimicrobial coating, includes the following steps：
(1) Fe is prepared3O4Adulterate TiO2Nanoparticle；
(2) by Fe3O4Adulterate TiO2Nanoparticle is dispersed in water, and moderate-speed mixer 25min, which is placed in microwave disperser, to be divided
Fe is made in scattered 25min3O4Adulterate TiO2Nanoparticle dispersion liquid；
(3) by water, Fe3O4Adulterate TiO2Nanoparticle dispersion liquid, titanium dioxide, 1,2 benzisothiazole-3-ketone polyoxy second
Allylic alkylation phenol ether through reaction is placed in moderate-speed mixer 35min in reaction vessel, and fluorine-containing lotion, ring are then added under stirring
Oxygen resin emulsion, melamine, carbodiimides, talcum powder, sodium polymethacrylate, aqueous color paste and alkanolamine, high speed
Trimethyl hydroxyl amylalcohol isobutyrate is added in the case where switching to moderate-speed mixer after stirring 55min, propylene glycol and high-carbon alcohol fatty acid ester are multiple
Close object, moderate-speed mixer 30min；
(4) it by the mixture prepared through filter cleaning, then measures, pack, storage saves.
The Fe3O4Adulterate TiO2The preparation of nanoparticle includes the following steps：
(1) by Ti (SO4)2It is dispersed in water, high-speed stirred 15min, ammonium hydroxide is added and adjusts solution to acidity, continues to stir
35min is filtered after standing 55min, dries to obtain solid after cleaning 4 times：
(2) solid that the step (1) obtains is dissolved with nitric acid solution, is filtered, collected filtrate, ten are added in filtrate
Dialkyl benzene sulfonic acids sodium adjusts soda acid to faintly acid with ammonium hydroxide；
(3) by Fe3O4It is dissolved in hydrochloric acid solution, the step (2) resulting solution is then added, adjust solution with ammonium hydroxide
To neutrality, moderate-speed mixer 100min then stands 55min, filters, and rinses, is repeated 5 times；
(4) by 500 DEG C of calcining 4h of the resulting solid of the step (3), grinding obtains Fe after natural cooling3O4Adulterate TiO2
Nanoparticle.
Wherein, the nitric acid is 0.7mol/L.
Embodiment 5：
A kind of antimicrobial coating, the antimicrobial coating include Fe3O4Adulterate TiO2Nanoparticle, the antimicrobial coating further include
The component of following parts by weight, 30 parts of fluorine-containing lotion, 30 parts of epoxy resin latex, 0.9 part of melamine, carbodiimides
0.9 part, 30 parts of talcum powder, 2 parts of sodium polymethacrylate, 28 parts of aqueous color paste, 2 parts of isobutyrate of trimethyl hydroxyl amylalcohol, the third two
1.5 parts of alcohol, 0.7 part of the fatty acid ester compounded object of higher alcohols, 30 parts of titanium dioxide, 0.3 part of polyoxyethylene alkylphenol base ether, 1,2 benzo
0.5 part of isothiazoline -3- ketone, 0.6 part of alkanolamine, 50 parts of water.
The Fe3O4Adulterate TiO2Fe in nanoparticle3O4Mass percentage is 0.07%.
Fe in the antimicrobial coating3O4Adulterate TiO2Nanoparticle mass percentage is 0.05%.
The Fe3O4Adulterate TiO2Nanoparticle is by Ti (SO4)2、Fe3O4, ammonium hydroxide, neopelex, nitric acid, salt
Acid and water are prepared by co-precipitation.
A kind of preparation process of antimicrobial coating, includes the following steps：
(1) Fe is prepared3O4Adulterate TiO2Nanoparticle；
(2) by Fe3O4Adulterate TiO2Nanoparticle is dispersed in water, and moderate-speed mixer 25min, which is placed in microwave disperser, to be divided
Fe is made in scattered 25min3O4Adulterate TiO2Nanoparticle dispersion liquid；
(3) by water, Fe3O4Adulterate TiO2Nanoparticle dispersion liquid, titanium dioxide, 1,2 benzisothiazole-3-ketone polyoxy second
Allylic alkylation phenol ether through reaction is placed in moderate-speed mixer 35min in reaction vessel, and fluorine-containing lotion, ring are then added under stirring
Oxygen resin emulsion, melamine, carbodiimides, talcum powder, sodium polymethacrylate, aqueous color paste and alkanolamine, high speed
Trimethyl hydroxyl amylalcohol isobutyrate is added in the case where switching to moderate-speed mixer after stirring 55min, propylene glycol and high-carbon alcohol fatty acid ester are multiple
Close object, moderate-speed mixer 25min；
(4) it by the mixture prepared through filter cleaning, then measures, pack, storage saves.
The Fe3O4Adulterate TiO2The preparation of nanoparticle includes the following steps：
(1) by Ti (SO4)2It is dispersed in water, high-speed stirred 15min, ammonium hydroxide is added and adjusts solution to acidity, continues to stir
35min is filtered after standing 60min, dries to obtain solid after cleaning 4 times：
(2) solid that the step (1) obtains is dissolved with nitric acid solution, is filtered, collected filtrate, ten are added in filtrate
Dialkyl benzene sulfonic acids sodium adjusts soda acid to faintly acid with ammonium hydroxide；
(3) by Fe3O4It is dissolved in hydrochloric acid solution, the step (2) resulting solution is then added, adjust solution with ammonium hydroxide
To neutrality, moderate-speed mixer 100min then stands 60min, filters, and rinses, is repeated 4 times；
(4) by 550 DEG C of calcining 5h of the resulting solid of the step (3), grinding obtains Fe after natural cooling3O4Adulterate TiO2
Nanoparticle.
Wherein, the nitric acid is 0.5mol/L.
Performance test
Comparative example 1 is using undoped with Fe3O4TiO2Nanoparticle replaces Fe3O4Adulterate TiO2, other components with reality
It is identical to apply example, its sterilizing activity is tested to embodiment 1- embodiment 5 and comparative example 1, by coating Tu obtained in 1m2PVC board
On, being placed in a space size is 1m3Closed transparent glass container in, and by container be placed in isolation sunlight have white heat
In the space of light, sterile culture medium is exposed to 1h after 1h, 12h and 72h in the test space, then and in air
The control medium of exposure 1h and not exposed aseptic culture medium are put in 36 DEG C of culture 48h in incubator together, count culture
Clump count on ware, and according in 5min in 100cm3The bacterial population to land on culture medium is equivalent to contained bacterium in 10L air
It counts and calculates 1m3Bacterial population (CFU/m in air3), it is recorded in table 1：
Table 1：
As shown in table, even if under visible light, embodiment can also show good bactericidal property relative to comparative example.
Claims (7)
1. a kind of antimicrobial coating, which is characterized in that the antimicrobial coating includes Fe3O4Adulterate TiO2Nanoparticle, the antibacterial apply
Layer further include following parts by weight component, 20-40 parts of fluorine-containing lotion, 20-40 parts of epoxy resin latex, melamine
0.1-1.5 parts, 0.1-1.5 parts of carbodiimides, 20-40 parts of talcum powder, 1-3 parts of sodium polymethacrylate, aqueous color paste 8-55
Part, 1-3 parts of amylalcohol isobutyrate of trimethyl hydroxyl, 0-2 parts of propylene glycol, fatty acid ester compounded object 0.5-1.0 parts of higher alcohols, titanium dioxide
20-40 parts, 0.2-0.4 parts of polyoxyethylene alkylphenol base ether, 1,2 0.4-0.6 parts of benzisothiazole-3-ketone, alkanolamine
0.5-0.7 parts, 40-60 parts of water.
2. a kind of antimicrobial coating according to claim 1, it is characterised in that：A kind of antibacterial according to claim 1
Coating, it is characterised in that：The antimicrobial coating further includes the component of following parts by weight, and 30 parts of fluorine-containing lotion, asphalt mixtures modified by epoxy resin
30 parts of fat liquor, 0.8 part of melamine, 0.9 part of carbodiimides, 33 parts of talcum powder, 2 parts of sodium polymethacrylate, aqueous color
25 parts of slurry, 2 parts of isobutyrate of trimethyl hydroxyl amylalcohol, 1.2 parts of propylene glycol, 0.8 part of the fatty acid ester compounded object of higher alcohols, titanium dioxide 28
Part, 0.3 part of polyoxyethylene alkylphenol base ether, 1,2 0.5 part of benzisothiazole-3-ketone, 0.6 part of alkanolamine, 50 parts of water.
3. a kind of antimicrobial coating according to claim 1, it is characterised in that：The Fe3O4Adulterate TiO2In nanoparticle
Fe3O4Mass percentage is 0.03-0.07%.
4. a kind of antimicrobial coating according to claim 1, it is characterised in that：Fe in the antimicrobial coating3O4Adulterate TiO2It receives
Rice corpuscles mass percentage is 0.01-0.05%.
5. a kind of antimicrobial coating according to claim 1, which is characterized in that the Fe3O4Adulterate TiO2Nanoparticle is by Ti
(SO4)2、Fe3O4, ammonium hydroxide, neopelex, nitric acid, hydrochloric acid and water are prepared.
6. a kind of preparation process for being used to prepare antimicrobial coating described in claim 1, which is characterized in that include the following steps：
(1) Fe is prepared3O4Adulterate TiO2Nanoparticle；
(2) by Fe3O4Adulterate TiO2Nanoparticle is dispersed in water, and moderate-speed mixer 10-30min, which is placed in microwave disperser, to be divided
Fe is made in scattered 10-30min3O4Adulterate TiO2Nanoparticle dispersion liquid；
(3) by water, Fe3O4Adulterate TiO2Nanoparticle dispersion liquid, titanium dioxide, 1,2 benzisothiazole-3-ketone polyoxyethylene alkane
Base phenol ether through reaction is placed in moderate-speed mixer 20-40min in reaction vessel, and fluorine-containing lotion, ring are then added under stirring
Oxygen resin emulsion, melamine, carbodiimides, talcum powder, sodium polymethacrylate, aqueous color paste and alkanolamine, high speed
Trimethyl hydroxyl amylalcohol isobutyrate, propylene glycol and high-carbon alcohol fatty acid ester are added in the case where switching to moderate-speed mixer after stirring 30-60min
Compound, moderate-speed mixer 10-30min；
(4) it by the mixture prepared through filter cleaning, then measures, pack, storage saves.
7. a kind of preparation process of antimicrobial coating according to claim 6, which is characterized in that the Fe3O4Adulterate TiO2It receives
The preparation of rice corpuscles includes the following steps
(1) by Ti (SO4)2It is dispersed in water, high-speed stirred 10-20min, ammonium hydroxide is added and adjusts solution to acidity, continues to stir
20-40min is filtered after standing 30-60min, dries to obtain solid after cleaning 3-5 times：
(2) solid for obtaining the step (1) nitric acid solution of 0.3-0.8mol/L dissolves, and filtering is collected filtrate, filtered
Neopelex is added in liquid, adjusts soda acid to faintly acid with ammonium hydroxide；
(3) by Fe3O4It is dissolved in hydrochloric acid solution, the step (2) resulting solution is then added, adjust solution into ammonium hydroxide
Property, moderate-speed mixer 60-120min then stands 30-60min, filters, rinse, repeats 3-5 times；
(4) by 450-550 DEG C of calcining 2-5h of the step (3) resulting solid, grinding obtains Fe after natural cooling3O4Doping
TiO2Nanoparticle.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111153440A (en) * | 2019-12-31 | 2020-05-15 | 陕西斯瑞新材料股份有限公司 | Fe for improving thermal emissivity3O4Preparation method and application of coating |
| WO2020187377A1 (en) * | 2019-03-19 | 2020-09-24 | ACT.Global R&D ApS | A transparent photocatalytic coating for in-situ generation of free radicals combating microbes, odors or organic compounds in visible light |
-
2018
- 2018-08-01 CN CN201810861109.2A patent/CN108864880A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020187377A1 (en) * | 2019-03-19 | 2020-09-24 | ACT.Global R&D ApS | A transparent photocatalytic coating for in-situ generation of free radicals combating microbes, odors or organic compounds in visible light |
| CN111153440A (en) * | 2019-12-31 | 2020-05-15 | 陕西斯瑞新材料股份有限公司 | Fe for improving thermal emissivity3O4Preparation method and application of coating |
| CN111153440B (en) * | 2019-12-31 | 2022-04-22 | 陕西斯瑞新材料股份有限公司 | Fe for improving thermal emissivity3O4Preparation method and application of coating |
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Application publication date: 20181123 |