CN106478903A - A kind of nanometer silver antimicrobial emulsion - Google Patents

A kind of nanometer silver antimicrobial emulsion Download PDF

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CN106478903A
CN106478903A CN201610820742.8A CN201610820742A CN106478903A CN 106478903 A CN106478903 A CN 106478903A CN 201610820742 A CN201610820742 A CN 201610820742A CN 106478903 A CN106478903 A CN 106478903A
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秦瑶
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    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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Abstract

The present invention relates to a kind of nanometer silver antimicrobial emulsion, is formed through emulsion polymerization by 56 parts of butyl acrylates, 13 parts of ethyl acrylates, 28 parts of methyl methacrylates, 4 parts of acrylic acid, 11 parts of hexafluorobutyl acrylates, 9 parts of acrylic acid trifluoro ethyl esters, 8 parts of fluorochemical monomer A, 12 parts of surface-modified nano titanium dioxide, 1.2 parts of sodium peroxydisulfates, 8 parts of hydroxy-ethyl acrylates, 6 parts of isopropyl naphthalene sulfonate, 4 parts of lauryl sodium sulfate, 4 parts of polysorbas20s, 5 parts of OP, 10,578 parts of deionized waters, 8 part of 4 vinyl aniline, 0.2 part of silver nitrate, 0.2 part of sodium borohydride.Nanometer silver antimicrobial emulsion of the present invention, its anti-microbial property are excellent, and the antibiotic rate to Escherichia coli and staphylococcus aureus is respectively 96% and more than 96.5%.

Description

A kind of nanometer silver antimicrobial emulsion
Technical field
The present invention relates to a kind of nanometer silver antimicrobial emulsion, belongs to functional high polymer material field.
Technical background
Presently used antiseptic mainly has natural antibacterial agent, organic antibacterial agent and inorganic antiseptic three major types.
Natural antibacterial agent derives from nature, the mainly extract in animals and plants, such as shitosan, propolis, nucleoprotamine, Mustard and allicin etc., are the mankind using earliest antiseptic.Natural antibacterial agent aboundresources, pair easy to use, safe and nontoxic Effect, but due to its poor heat resistance, stability is poor, service life is short, do not possess broad-spectrum long-acting, production is originated and extraction level Limited the problems such as, it is very limited in the application, can not still realizes mass market.
Organic antibacterial agent be with organic acid, phenols, quaternary ammonium salt, organic amine, benzimidazole, OIT The organic matters such as class, formaldehyde releaser are the antiseptic of antimicrobial component, and wherein quaternary ammonium salt and quaternary alkylphosphonium salt compound antiseptic of birdsing of the same feather flock together is The focus that studies at present.Organic antibacterial agent abundance, sterilizing power are strong, prompt effect is good, antibacterial range is wide, anti-discoloration ability strong, But security is poor, poor heat resistance, easily ooze out, easily decompose, easily migrate, to be also easy to produce microorganism drug resistance, toxicity larger, not washable Wash, service life is short, for a long time using harmful, which is using there is significant limitation.
Inorganic antiseptic is the ability of the antibacterial or sterilization having using the metals such as silver, zinc, copper and its ion itself, leads to The methods such as physical absorption, ion exchange and multilayer coating structure are crossed, by the metals such as silver, zinc, copper and its ion load in zeolite, phosphate Deng on porous material, processed obtained class antiseptic.
Nano silver antimicrobials are a kind of new and effective antiseptics, and due to its skin effect, antibacterial ability is micron order silver granuel More than 200 times of son, anti-microbial property is far longer than traditional silver-series antibacterial agent, and its exploitation is silver-series antibacterial agent from now on application Important development direction.
Water-borne Acrylic Coating has that good film-forming property, application property be good, film alkali resistance and colour retention are good and pollution-free The advantages of, obtain at present and be widely applied.However, easy embrittlement under esters of acrylic acid product cryogenic conditions, heat-resisting quantity is poor, In coating application, most obvious shortcoming is exactly that high temperature after-tacks, and causes stain resistance to decline, and resistance to water and weatherability are also poor, this A little factors cause its range to be subject to certain restrictions.In order to obtain the acrylic coating of excellent performance, people are one after another mesh Light invests the modification to acrylic resin.In recent years, acrylic resin is modified using fluorochemical monomer, propylene can be kept The original advantage of acid ester copolymer, gives the spies such as its excellent weatherability, resistance to water, oil resistivity, heat resistance and stain resistance again Point, thus be with a wide range of applications.
Additionally, organic-inorganic nanocomposite has the advantage of organic and inorganic materials concurrently, mutually cover the shortage, can use In the study on the modification of coating, plastics, rubber etc., in order to improve the performance of material.Nano-titania particle low cost, source Extensively, it is introduced in polymeric system as a kind of functional component, the wearability of coating, weatherability, resistance to not only can be improved Solvent borne and uvioresistant photosensitiveness, and enable surface to form nanostructured, improve the Water-proof and oil-proof performance on surface.Therefore will Nano-titania particle is introduced in fluorine richness polyacrylate dispersion, prepares inorganic-organic hybridization nano titanium dioxide/fluorine-containing Polymer is one of new direction of following acrylic coating development.
Content of the invention
It is an object of the invention to provide a kind of fluorinated acrylate nanometer silver antimicrobial emulsion, by fluorine, nano titanium oxide Modification acrylate, and formation Nano Silver on acrylate polymer strand altogether, is obtained inorganic-organic hybridization nano dioxy Change titanium/fluorine-containing antibacterial polymer.
For achieving the above object, technical scheme below present invention employs:
A kind of nanometer silver antimicrobial emulsion:In terms of mass parts, by 56 parts of butyl acrylates, 13 parts of ethyl acrylates, 28 parts of first Base methyl acrylate, 4 parts of acrylic acid, 11 parts of hexafluorobutyl acrylates, 9 parts of acrylic acid trifluoro ethyl esters, 8 parts of fluorochemical monomer A, 12 parts Surface-modified nano titanium dioxide, 1.2 parts of sodium peroxydisulfates, 8 parts of hydroxy-ethyl acrylates, 6 parts of isopropyl naphthalene sulfonate, 4 part 12 Sodium alkyl sulfate, 4 parts of Tween-20s, 5 parts of OP-10,578 parts of deionized waters, 8 parts of 4- vinyl aniline, 0.2 part of silver nitrate, 0.2 Part sodium borohydride is formed through emulsion polymerization;
The structural formula of described fluorochemical monomer A is as shown in Equation 1:
The preparation method of fluorochemical monomer A is:In the three-neck flask equipped with reflux condensing tube and constant pressure funnel, formula is added The 3- butene-1-ol of amount and appropriate absolute ether, are slowly added dropwise the Hexafluoropropylene third of 3- butene-1-ol equimolar amounts under room temperature Alkane dimer, reacts about 12h under agitation, after removing the ether in reactant mixture, then obtains fluorochemical monomer through vacuum distillation A.
Described surface-modified nano titanium dioxide is obtained by following methods:
Successively by mass ratio for 1: 10: 0.2: 0.3 particle diameter be the titanium dioxide of 30~50nm, absolute ethyl alcohol, 3- (methyl Acryloyl-oxy) propyl trimethoxy silicane, ten trifluoro octyl group trimethoxy silanes are put in there-necked flask, add vinegar acid for adjusting pH =5.5~6.5, stirring reaction after 4 hours at 70 DEG C, cooling;It is centrifuged at a high speed repeatedly 5 times by absolute ethyl alcohol, removes Unnecessary coupling agent;Filter cake drying, grind, sieve, obtaining final product modified nano-titanium dioxide powder;
A kind of preparation method of described nanometer silver antimicrobial emulsion is:
A, 508 parts of deionized waters and 12 parts of surface-modified nano titanium dioxide are added equipped with temperature measuring equipment, electric stirring In device, the reactor of condensing unit, stirring is started, after stirring evenly, add 6 parts of isopropyl naphthalene sulfonate, 4 parts of dodecyl sulphates Sodium, 4 parts of Tween-20s, 5 parts of OP-10, high-speed stirred 30min, emulsion dispersion;
B, by 56 parts of butyl acrylates, 13 parts of ethyl acrylates, 28 parts of methyl methacrylates, 4 parts of acrylic acid, 11 part third Olefin(e) acid hexafluoro butyl ester, 9 parts of acrylic acid trifluoro ethyl esters, 8 parts of fluorochemical monomer A, 8 parts of 4- vinyl aniline are stirred into mixing list Body;30 parts of deionized waters are dissolved into initiator solution with 1.2 parts of sodium peroxydisulfates;
C, in reactor add 1/4 mix monomer, high-speed stirred emulsification 30min after, when being heated to 60 DEG C, plus Enter 1/2 initiator solution, when 80 DEG C are warming up to, synchronously the remaining mix monomer of dropping and initiator solution, keep reaction At 80 DEG C, about 3h is dripped temperature;
After d, monomer and initiator are added, continue to react 1h at 90 DEG C, less than 40 DEG C are cooled to, add 0.2 part of silver nitrate With the solution of 20 parts of deionized waters, after stirring, the solution of 0.2 part of sodium borohydride and 20 parts of deionized waters is rapidly added, is entered Row reduction reaction;200 mesh sieves are crossed, obtains final product nanometer silver antimicrobial emulsion.
Although silane coupler preferably can be combined with nano titanium oxide, its organo-functional group chain is shorter, is coupled Agent molecule chain to the masking of nano titanium oxide surface hydroxyl not exclusively, and nano titanium oxide surface hydroxyl do not have completely with idol Connection agent molecule reacts, so that nano-titania particle cannot be compatible well with non-polar organic solvent, monomer, Easily reunite in polymer emulsion.Silicon fluoride coupling agent and silane coupler modified synergic nano-titania particle, fluoroalkyl can Effectively reduce the surface tension of nano-particle, promote stablizing for nano-particle, nano-particle in emulsion polymerization process can be avoided Reunion;Additionally, by the C=C double bond of silane coupler, polymer is formed in nanoparticle surface, form inorganic-organic multiple Condensation material, enhances emulsion film strength, the performance such as water-fast.
Fluorine has especially strong hydrophobicity, and fluoro-containing group is easily enriched in the surface of film in film forming, is formed tight hydrophobic Layer, and the fluorine silicone couplet of nano titanium oxide surface grafting, can effectively weaken the nanometer titanium dioxide positioned at emulsion film surface The defect that titanium particle causes emulsion film hydrophobicity deficiency because of the surface unreacted hydroxyl group absorption moisture in air for containing.
Nanometer silver antimicrobial emulsion of the present invention, its anti-microbial property are excellent, to Escherichia coli and the antibacterial of staphylococcus aureus Rate is respectively 96% and more than 96.5%.
Nano titanium oxide is good with its activity height, heat endurance and heat-resist, continuation length, safe, prompt effect The advantages of, become inorganic antiseptic of greatest concern.Nano titanium oxide to Pseudomonas aeruginosa, Escherichia coli, gold-coloured staphylococci, Salmonella etc. all has very strong sterilizing ability, forms antibacterial cooperative effect with Nano Silver.
The present invention is modified to polyacrylate with silicon fluoride coupling agent, fluorine monomer, nano titanium oxide, is improved poly- The performance such as heat-resisting, water-fast and weather-proof of acrylic acid ester emulsion.
Specific embodiment
Below by specific embodiment, the invention will be further described:
A kind of nanometer silver antimicrobial emulsion, in terms of mass parts, by 56 parts of butyl acrylates, 13 parts of ethyl acrylates, 28 parts of first Base methyl acrylate, 4 parts of acrylic acid, 11 parts of hexafluorobutyl acrylates, 9 parts of acrylic acid trifluoro ethyl esters, 8 parts of fluorochemical monomer A, 12 parts Surface-modified nano titanium dioxide, 1.2 parts of sodium peroxydisulfates, 8 parts of hydroxy-ethyl acrylates, 6 parts of isopropyl naphthalene sulfonate, 4 part 12 Sodium alkyl sulfate, 4 parts of Tween-20s, 5 parts of OP-10,578 parts of deionized waters, 8 parts of 4- vinyl aniline, 0.2 part of silver nitrate, 0.2 Part sodium borohydride is formed through emulsion polymerization
Fluorochemical monomer A is made up with dimerization of hexafluoropropene oxide precursor reactant of 3- butene-1-ol, and other component substance are city Sell product.
The preparation method of fluorochemical monomer A is:In the three-neck flask equipped with reflux condensing tube and constant pressure funnel, formula is added The 3- butene-1-ol of amount and appropriate absolute ether, are slowly added dropwise the Hexafluoropropylene third of 3- butene-1-ol equimolar amounts under room temperature Alkane dimer, reacts about 12h under agitation, after removing the ether in reactant mixture, then obtains fluorochemical monomer through vacuum distillation A.
Reaction equation is as follows:
Described sodium peroxydisulfate is initiators for polymerization, hydroxy-ethyl acrylate is self-cross linking monomer.
Described isopropyl naphthalene sulfonate, lauryl sodium sulfate, Tween-20, OP-10 are emulsifying agent.
Nano titanium oxide is a kind of very high function fine inorganic material of added value.Because its have good weatherability, The features such as chemical resistance, anti-uv-ray are strong, and be widely used.But as the surface energy of nanometer particle is high, hold Easily reunite, offspring is formed, the shortcomings of infiltrating with dispersion stabilization difference is difficult in organic phase, it is impossible to it is to show The nano-meter characteristics such as satisfied big specific area effect, bulk effect and quantum size effect.Therefore in order to improve nano titanium oxide With the compatibility of organic system and its dispersion stabilization in organic system, the compound system that adds nano titanium oxide is improved Combination property, it is necessary to which surface modification is carried out to which, by change nano titanium oxide surface physico-chemical property, improve its with organic The compatibility and adhesion of molecule.
Coupling agent modified nano-particle is, in nanoparticle surface, chemical coupling reaction occurs, coupling agent and nano-particle it Between in addition to Van der Waals force, hydrogen bond or coordinate bond interact, the combination of also ionic bond or covalent bond.Nanoparticle surface warp Good compatibility can be produced with organic matter after coupling agent treatment.Coupling agent molecule must possess two kinds of groups, a kind of and nothing Machine thing nanoparticle surface carries out chemical reaction;Another kind of (organo-functional group) has reactivity with organic matter matrix.3- (methyl Acryloyl-oxy) can be anti-with the hydroxyl on nano titanium oxide surface after methoxy silane hydrolysis in propyl trimethoxy silicane molecule Should, so that coupling agent molecule is fixed on nanoparticle surface;Thiazolinyl in molecule can be polymerized instead with C=C double bond monomer Should, in nanoparticle surface graft polymers.The siloxy of silane coupler can occur grafting anti-with titanium dioxide surface hydroxyl Should, increase space repulsion, prevent the reunion of titanium dioxide, improve the interface compatibility of inorganic phase and organic phase, while silane idol The polymerizable functional group of connection agent can play the dual property of inorganic-organic composite material with other unsaturated monomer reactions.But silicon The coupling agent modified nano titanium oxide of alkane has the disadvantage that:Coupling agent molecule chain is covered not to nano titanium oxide surface hydroxyl Completely, nano titanium oxide surface hydroxyl is not reacted with coupling agent molecule completely, so that nano titanium oxide grain Son cannot be compatible well with non-polar organic solvent, monomer, easily reunites in polymer emulsion;The nanometer two introduced in emulsion The hydroxyl for not reacting with coupling agent or covering is contained on Titanium particles surface, and film hydrophobicity can be caused not enough.
By silanol key and the hydroxyl reaction on nano titanium oxide surface after the hydrolysis of ten trifluoro octyl group trimethoxy silanes, with Chemical bond is stably distributed in nanoparticle surface, can significantly decrease the surface tension of nano titanium oxide, strengthens nanometer Dispersiveness of the titanium dioxide in water, stability, improve the compatibility of nano titanium oxide and fluorine-containing organic monomer, and favorably In fluorochemical monomer nanoparticle surface glycerol polymerization.
Surface-modified nano titanium dioxide process is:Successively by mass ratio for 1: 10: 0.2: 0.3 particle diameter be 30~ The titanium dioxide of 50nm, absolute ethyl alcohol, 3- (methacryloxypropyl) propyl trimethoxy silicane, ten trifluoro octyl group trimethoxy silicon Alkane is put in there-necked flask, is added acetic acid and is adjusted pH=5.5~6.5, stirring reaction after 4 hours at 70 DEG C, cooling;By no Water-ethanol is centrifuged at a high speed 5 times repeatedly, removes unnecessary coupling agent;Filter cake drying, grind, sieve, obtaining final product modified Nano Titania powder.
A kind of preparation method of the nano-titanium dioxide modified acrylate nanometer silver antimicrobial emulsion of fluorine is:
A, 508 parts of deionized waters and 12 parts of surface-modified nano titanium dioxide are added equipped with temperature measuring equipment, electric stirring In device, the reactor of condensing unit, stirring is started, after stirring evenly, add 6 parts of isopropyl naphthalene sulfonate, 4 parts of dodecyl sulphates Sodium, 4 parts of Tween-20s, 5 parts of OP-10, high-speed stirred 30min, emulsion dispersion;
B, by 56 parts of butyl acrylates, 13 parts of ethyl acrylates, 28 parts of methyl methacrylates, 4 parts of acrylic acid, 11 part third Olefin(e) acid hexafluoro butyl ester, 9 parts of acrylic acid trifluoro ethyl esters, 8 parts of fluorochemical monomer A are stirred into mix monomer;30 parts of deionized waters with 1.2 parts of sodium peroxydisulfates are dissolved into initiator solution;
C, in reactor add 1/4 mix monomer, high-speed stirred emulsification 30min after, when being heated to 60 DEG C, plus Enter 1/2 initiator solution, when 80 DEG C are warming up to, synchronously the remaining mix monomer of dropping and initiator solution, keep reaction At 80 DEG C, about 3h is dripped temperature;
After d, monomer and initiator are added, continue to react 1h at 90 DEG C, less than 40 DEG C are cooled to, add 0.2 part of silver nitrate With the solution of 20 parts of deionized waters, after stirring, the solution of 0.2 part of sodium borohydride and 20 parts of deionized waters is rapidly added, is entered Row reduction reaction;200 mesh sieves are crossed, obtains final product nanometer silver antimicrobial emulsion.
The rotating speed of described high-speed stirred is 5000-8000 rev/min.
Embodiment 1:
The synthesis of fluorochemical monomer A
In the three-neck flask equipped with reflux condensing tube and constant pressure funnel, 3- butene-1-ol and the 500mL of 0.5mol are added Absolute ether, is slowly added dropwise 0.5mol dimerization of hexafluoropropene oxide body, reacts about 12h under agitation under room temperature, except dereaction is mixed After ether in compound, then fluorochemical monomer A is obtained through vacuum distillation.
Embodiment 2:
Surface-modified nano titanium dioxide process:
Successively by 18 parts of titanium dioxide that particle diameter is 30~50nm, 220 parts of absolute ethyl alcohol, 3- (methacryloxypropyl) propyl group 8 parts of trimethoxy silane, 6 parts of ten trifluoro octyl group trimethoxy silane are put in there-necked flask, add acetic acid adjust pH=5.5~ 6.5, stirring reaction after 4 hours at 70 DEG C, cooling;It is centrifuged at a high speed repeatedly 5 times by absolute ethyl alcohol, removes unnecessary idol Connection agent;Filter cake drying, grind, sieve, obtaining final product modified nano-titanium dioxide powder.
Embodiment 3:
A kind of preparation method of nanometer silver antimicrobial emulsion is:
A, 508 parts of deionized waters and 12 parts of surface-modified nano titanium dioxide are added equipped with temperature measuring equipment, electric stirring In device, the reactor of condensing unit, stirring is started, after stirring evenly, add 6 parts of isopropyl naphthalene sulfonate, 4 parts of dodecyl sulphates Sodium, 4 parts of Tween-20s, 5 parts of OP-10, high-speed stirred 30min, emulsion dispersion;
B, by 56 parts of butyl acrylates, 13 parts of ethyl acrylates, 28 parts of methyl methacrylates, 4 parts of acrylic acid, 11 part third Olefin(e) acid hexafluoro butyl ester, 9 parts of acrylic acid trifluoro ethyl esters, 8 parts of fluorochemical monomer A are stirred into mix monomer;30 parts of deionized waters with 1.2 parts of sodium peroxydisulfates are dissolved into initiator solution;
C, in reactor add 1/4 mix monomer, high-speed stirred emulsification 30min after, when being heated to 60 DEG C, plus Enter 1/2 initiator solution, when 80 DEG C are warming up to, synchronously the remaining mix monomer of dropping and initiator solution, keep reaction At 80 DEG C, about 3h is dripped temperature;
After d, monomer and initiator are added, continue to react 1h at 90 DEG C, less than 40 DEG C are cooled to, add 0.2 part of silver nitrate With the solution of 20 parts of deionized waters, after stirring, the solution of 0.2 part of sodium borohydride and 20 parts of deionized waters is rapidly added, is entered Row reduction reaction;200 mesh sieves are crossed, obtains final product nanometer silver antimicrobial emulsion.
Using the method for plate culture count, nanometer silver antimicrobial emulsion of the present invention is tested to Escherichia coli and staphylococcus aureus Antibacterial effect.Concrete operation step is:It is 5.0 × 10 to select concentration5The dilution of individual or so thalline/milliliter, used as test With bacterium solution, take 10 milliliters and be added to containing 25 milliliters of culture mediums that (its formula is:2.0 grams of peptone, 1.0 grams of Yeast mannan, chlorination 2.0 grams of sodium, 3.0 grams of agar-agar and 220 milliliters of distilled water) conical flask in, equally take 3 conical flasks, two check experiments, another The individual complex emulsions for the present invention;Nanometer silver emulsion addition of the present invention is 2g, control group 1:Addition does not contain nano silver particles, Other components are identical;Control group 2:Without any material (blank);3 conical flasks are placed on 40 revs/min of shaking tables, constant temperature 37 ± 1 DEG C, cultivate 24 hours, then take a certain amount of bacterium solution and be laid in agar Nutrient medium, living after cultivating 24 hours at 37 ± 1 DEG C Bacterium counts, and then calculates antibiotic rate.
By the method for testing, nanometer silver antimicrobial emulsion of the present invention is to Escherichia coli and the antibiotic rate of staphylococcus aureus Respectively 96% and more than 96.5%.

Claims (1)

1. a kind of nanometer silver antimicrobial emulsion, it is characterised in that:In terms of mass parts, by 56 parts of butyl acrylates, 13 parts of acrylic acid second Ester, 28 parts of methyl methacrylates, 4 parts of acrylic acid, 11 parts of hexafluorobutyl acrylates, 9 parts of acrylic acid trifluoro ethyl esters, 8 parts fluorine-containing Monomer A, 12 parts of surface-modified nano titanium dioxide, 1.2 parts of sodium peroxydisulfates, 8 parts of hydroxy-ethyl acrylates, 6 parts of isopropyl naphthalene sulfonic acid Sodium, 4 parts of lauryl sodium sulfate, 4 parts of Tween-20s, 5 parts of OP-10,578 parts of deionized waters, 8 parts of 4- vinyl aniline, 0.2 part Silver nitrate, 0.2 part of sodium borohydride are formed through emulsion polymerization;
The structural formula of described fluorochemical monomer A is as shown in Equation 1:
The preparation method of fluorochemical monomer A is:In the three-neck flask equipped with reflux condensing tube and constant pressure funnel, formula ratio is added 3- butene-1-ol and appropriate absolute ether, are slowly added dropwise the HFPO two of 3- butene-1-ol equimolar amounts under room temperature Aggressiveness, reacts about 12h under agitation, after removing the ether in reactant mixture, then obtains fluorochemical monomer A through vacuum distillation;
Described surface-modified nano titanium dioxide is obtained by following methods:
Successively by mass ratio for 1: 10: 0.2: 0.3 particle diameter be the titanium dioxide of 30~50nm, absolute ethyl alcohol, 3- (metering system Acyl-oxygen) propyl trimethoxy silicane, ten trifluoro octyl group trimethoxy silanes are put in there-necked flask, add acetic acid and adjust pH= 5.5~6.5, stirring reaction after 4 hours at 70 DEG C, cooling;It is centrifuged at a high speed repeatedly 5 times by absolute ethyl alcohol, removes many Remaining coupling agent;Filter cake drying, grind, sieve, obtaining final product modified nano-titanium dioxide powder;
A kind of preparation method of described nanometer silver antimicrobial emulsion is:
A, by 508 parts of deionized waters and 12 parts of surface-modified nano titanium dioxide add equipped with temperature measuring equipment, electric mixing device, In the reactor of condensing unit, start stirring, add after stirring evenly 6 parts of isopropyl naphthalene sulfonate, 4 parts of lauryl sodium sulfate, 4 parts Tween-20,5 parts of OP-10, high-speed stirred 30min, emulsion dispersion;
B, by 56 parts of butyl acrylates, 13 parts of ethyl acrylates, 28 parts of methyl methacrylates, 4 parts of acrylic acid, 11 parts of acrylic acid Hexafluoro butyl ester, 9 parts of acrylic acid trifluoro ethyl esters, 8 parts of fluorochemical monomer A, 8 parts of 4- vinyl aniline are stirred into mix monomer;30 Part deionized water is dissolved into initiator solution with 1.2 parts of sodium peroxydisulfates;
C, in reactor add 1/4 mix monomer, high-speed stirred emulsification 30min after, when being heated to 60 DEG C, add 1/ 2 initiator solution, when being warming up to 80 DEG C, synchronously the remaining mix monomer of dropping and initiator solution, keep reaction temperature At 80 DEG C, about 3h is dripped;
After d, monomer and initiator are added, continue to react 1h at 90 DEG C, less than 40 DEG C are cooled to, add 0.2 part of silver nitrate and 20 The solution of part deionized water, after stirring, is rapidly added the solution of 0.2 part of sodium borohydride and 20 parts of deionized waters, carries out also Former reaction;200 mesh sieves are crossed, obtains final product nanometer silver antimicrobial emulsion.
CN201610820742.8A 2016-08-31 2016-08-31 A kind of nanometer silver antimicrobial emulsion Pending CN106478903A (en)

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CN107787965A (en) * 2017-10-25 2018-03-13 浏阳市湘杰机械制造有限公司 A kind of environmentally friendly fungus and mildew resistance spray
CN111378340A (en) * 2020-04-10 2020-07-07 河南功能高分子膜材料创新中心有限公司 Preparation method of modified polyacrylic resin and modified polyacrylic resin
CN111467247A (en) * 2020-04-24 2020-07-31 中国人民解放军总医院 Preparation method of nano-silver/PMMA (polymethyl methacrylate) denture base composite material
CN111574871A (en) * 2020-04-23 2020-08-25 武汉中科先进技术研究院有限公司 Modified fluorosilane composite sol, preparation method thereof, coating containing modified fluorosilane composite sol, and preparation method and application of coating
CN111826017A (en) * 2020-07-13 2020-10-27 同曦集团有限公司 Antibacterial and antiviral composition, antibacterial and antiviral coating and container
CN114410175A (en) * 2021-12-11 2022-04-29 东来涂料技术(上海)股份有限公司 High-wear-resistance coating for automotive interior parts and preparation method thereof

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107787965A (en) * 2017-10-25 2018-03-13 浏阳市湘杰机械制造有限公司 A kind of environmentally friendly fungus and mildew resistance spray
CN107787965B (en) * 2017-10-25 2021-03-09 浏阳市湘杰机械制造有限公司 Environment-friendly sterilization mildew-proof spray
CN111378340A (en) * 2020-04-10 2020-07-07 河南功能高分子膜材料创新中心有限公司 Preparation method of modified polyacrylic resin and modified polyacrylic resin
CN111574871A (en) * 2020-04-23 2020-08-25 武汉中科先进技术研究院有限公司 Modified fluorosilane composite sol, preparation method thereof, coating containing modified fluorosilane composite sol, and preparation method and application of coating
CN111467247A (en) * 2020-04-24 2020-07-31 中国人民解放军总医院 Preparation method of nano-silver/PMMA (polymethyl methacrylate) denture base composite material
CN111826017A (en) * 2020-07-13 2020-10-27 同曦集团有限公司 Antibacterial and antiviral composition, antibacterial and antiviral coating and container
CN114410175A (en) * 2021-12-11 2022-04-29 东来涂料技术(上海)股份有限公司 High-wear-resistance coating for automotive interior parts and preparation method thereof
CN114410175B (en) * 2021-12-11 2023-11-10 东来涂料技术(上海)股份有限公司 High-wear-resistance coating for automotive upholstery and preparation method thereof

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Application publication date: 20170308