CN106634512A - Super-amphiphobic silver series anti-microbial compound hybridizing anti-corrosion coating - Google Patents
Super-amphiphobic silver series anti-microbial compound hybridizing anti-corrosion coating Download PDFInfo
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- 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3802—Low-molecular-weight compounds having heteroatoms other than oxygen having halogens
- C08G18/3804—Polyhydroxy compounds
- C08G18/3812—Polyhydroxy compounds having fluorine atoms
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/015—Biocides
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
- C09D5/10—Anti-corrosive paints containing metal dust
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The invention discloses a super-amphiphobic silver series anti-microbial compound hybridizing anti-corrosion coating which is prepared from the following raw materials: perfluoroalkyl alcohol, methyl isobutyl ketone, HDI trimer, methyl methacrylate, styrene, hydroxyethyl methylacrylate, trifluorooctyl methacrylate, benzoyl peroxide, methanol silica sol, propylene glycol methyl ether acetate, a defined amount of 5% ammonium hydroxide, a defined amount of methyl-tri-(butanone-oxime) silane, a defined amount of methyl hydrogen silicone oil, a defined amount of 10% dibutyltin dilaurate, a dispersing agent, a flatting agent, a de-foaming agent, a defined amount of n-butyl acetate, silver nitrate, graphene oxide, diallyldimethylammonium chloride and a defined amount of deionized water. The super-amphiphobic coating prepared according to the invention has the advantages of excellent non-viscosity, heat resistance, corrosion resistance, cold and heat resistance, mold resistance and easiness in implementation. The coating is high in adhesive force, is difficult to fall off, is long in service life and is higher in practical use value.
Description
Technical field
The present invention relates to technical field of coatings, more particularly to a kind of super-amphiphobic silver system antibacterial composite hybridization corrosion resistant coating.
Background technology
Wettability is a key property of the surface of solids, it is conventionally believed that the microstructure of the surface of solids and chemical group
The wettability that in pairs it is shown plays a key effect.The wettability of the surface of solids rises in daily life and industrial and agricultural production
Critically important effect, such as washing, printing and dyeing, the dispersion of coating, the use of lubricating oil and the infiltration of skin care item.Current people
Do not get wet this, and the phenomenon that water droplet can be tumbled with oneself is referred to as super-hydrophobic phenomenon, and the surface with this property is claimed
For super hydrophobic surface, research worker is more for the research of super hydrophobic coating, but the type coating be often easily stained with oil stain and compared with
Hardly possible is removed, therefore greatly limit the application and popularization of the type coating.Double open coats are because it is for alienation while water and oil
Effect, simple super-hydrophobic coat of holding one's breath is easier to be applied in the middle of daily life and commercial production.But it is existing at present
Super-hydrophobic oleophobic coating preparation method has the following disadvantages：Need special installation（Plasma, laser ablation）, be unfavorable for large area
Construction, has particular/special requirement to ground, is only applicable to particular surface, and universal complex forming technology, with high costs, therefore seriously
Limit the extensive application of such material.
Xu Runbin exists《The preparation of super-hydrophobic/oleophobic coating and research》Nanometer is prepared in one text by conventional grinding methods
Aluminium sesquioxide particle, nano-silicon dioxide particle is prepared for using sol-gel process, is distinguished using fluorine-containing silane coupler
Surface grafting process is carried out to both, the nanoparticle and micron particle of surface fluorine modification has been obtained as color stuffing, next is adopted
With polytype acrylic monomerss a kind of fluorine-containing Hydroxylated acrylic resin is prepared as the main resin of binding agent, selection perfluoroalkyl
Ethanol and hexamethylene diisocyanate trimer prepare a kind of fluorine-containing isocyanate curing agent, and as a result paint is matched somebody with somebody in surface by mixing
The acroleic acid polyurethane varnish paint film property of preparation is good, adhesion 1 grade, pliability 1mm, impact 50cm, hardness 2H, for water
Static contact angle reach as high as 104 °, finally obtained nanometer, micron particle are scattered in fluorine-containing Hydroxylated acrylic resin,
Adjustment pigment and nano/micrometre particle ratio, and be equipped with dispersant, anti-settling auxiliary agent and firming agent be obtained it is various super thin
Water-oleophobic coating, testing result show coating there is preferable adhesive force, pliability and paint film intensity, now film for water,
The static contact angle of Oleum Brassicae campestriss and aircraft fluid is respectively 154 °, 100 ° and 94 °, illustrates that the coating shows to water and oil
Good alienation effect, although the preparation method proposed in this article has certain effect in terms of hydrophobic and oleophobic, but
The contact angle to oil is not reaching to more than 150 °, and the intensity of coating, wearability, durability, stability and mechanical performance one
As, actual use demand is can not meet, limit the commercial Application of super-amphiphobic coating.
The content of the invention
The object of the invention is exactly to make up the defect of prior art, there is provided a kind of super-amphiphobic silver system antibacterial composite hybridization is resistance to
Etching ground.
The present invention is achieved by the following technical solutions：
A kind of super-amphiphobic silver system antibacterial composite hybridization corrosion resistant coating, is made up of the raw material of following weight portion：Perfluoroalkyl
Ethanol 32-35, methyl iso-butyl ketone (MIBK) 40-50, HDI trimer 90-100, methyl methacrylate 30-35, styrene 20-23,
Hydroxyethyl methylacrylate 8.5-9, the trifluoro monooctyl ester 17-19 of methacrylic acid ten, benzoyl peroxide 0.6-0.8, methanol silicon are molten
Glue 25-28, propylene glycol methyl ether acetate 25-26, appropriate 5% ammonia, appropriate methyl tributanoximo silane, methyl hydrogen silicon
Oily appropriate, 10% dibutyl tin laurate is appropriate, dispersant 0.6-1, levelling agent 0.6-0.8, defoamer 0.4-0.6, acetic acid fourth
Appropriate ester, silver nitrate 2.3-2.5, graphene oxide 5.5-6, diallyldimethylammonium chloride 0.4-0.6, deionized water are fitted
Amount.
A kind of super-amphiphobic silver system antibacterial composite hybridization corrosion resistant coating, is made up of step in detail below：
（1）Perfluoroalkyl ethanol is mixed with the methyl iso-butyl ketone (MIBK) of butyl acetate, 2/3 times of amount, in being added to reaction bulb, starts to rise
Temperature is simultaneously slowly stirred to perfluoroalkyl ethanol and is completely dissolved, and instills the dibutyl tin laurate of 8-10 drops 10%, and liter high-temperature is extremely
After 70 DEG C, the mixed liquor of Deca HDI trimer and butyl acetate, it is ensured that the completion of dropping in 1h is stepped up temperature to 90 DEG C,
Cooling down is standby as component A to room temperature after insulation 2-3h；
（2）Appropriate butyl acetate is added to into vessel in heating to the insulation 20min that flows back, then by methyl methacrylate, benzene second
The mixing of alkene, hydroxyethyl methylacrylate, remaining methyl iso-butyl ketone (MIBK), 80% benzoyl peroxide and butyl acetate, wherein vinegar
Acid butyl ester is 3 with the volume ratio of methyl iso-butyl ketone (MIBK):1, the butyl acetate of above-mentioned backflow insulation is slowly dropped to after stirring and dissolving
In solution, it is ensured that completion of dropping in 1.5h, the trifluoro monooctyl ester of methacrylic acid ten is then rapidly added, rises high-temperature to 95 DEG C of backflows
Insulation 2h, is then disposably added to 10% benzoyl peroxide and appropriate butyl acetate mixing in container, insulation reaction 1-
After 1.5h remaining benzoyl peroxide and appropriate butyl acetate are mixed again and disposably added, insulation reaction 1-1.5h, with
After be cooled to 50 DEG C, seal standby；
（3）Silver nitrate is added in deionized water the solution for making that concentration is 2wt%, in addition graphene oxide deionization is added to into
In water, ultrasonic disperse makes the dispersion liquid of 0.1wt%, then diallyldimethylammonium chloride ultrasonic agitation is added in dispersion liquid,
Stir and add silver nitrate solution in the backward mixed liquor, be placed in after stirring in hydrothermal reaction kettle, at 160 DEG C 3- is reacted
4h, is cooled to centrifugation after room temperature, and by product dehydrated alcohol and deionized water wash 3 times, is placed in baking oven after cleaning
Drying for standby at 90 DEG C；
（4）Methanol Ludox is placed in the container that bath temperature is 60 DEG C, total system quality is slowly added under agitation
Fraction is 12% methyl tributanoximo silane, and isothermal reaction 1h adds total system mass fraction for 3% Methyl Hydrogen Polysiloxane Fluid
Continue to react 1h, be subsequently adding after propylene glycol methyl ether acetate mix homogeneously and be transferred in rotary evaporator, vacuum distillation is removed
Methanol, obtains the scattered hydrophobically modified Ludox of propylene glycol methyl ether acetate；
（5）By step（3）The product of preparation is added to step（4）In, being placed in fully shaking in ultrasonator uniformly, then will be mixed
Compound is added to step（2）It is slowly stirred in the product of preparation to being uniformly dispersed, adds dispersant, levelling agent and defoamer at a high speed
Stirring 30-50min, rotating speed is controlled to 1000-1200r/min, and then ultrasonic disperse 30-40min, then continues to high-speed stirred
20-30min, rotating speed is controlled to 700r/min, obtains component B, then by component A and component B according to mass ratio 1：3.2 mixing,
Room temperature is placed 10-15min and carries out ripening, is adjusted to suitable viscosity with ethyl acetate and is sprayed or brush after surface of the work, surface drying
The baking-curing at 80 DEG C.
It is an advantage of the invention that：Polyurethane resin has good adhesive force, mechanical endurance and toughness, and film is acidproof
Alkali, chemical-resistant resistance, saline solution etc., film can in -50 DEG C of -120 DEG C of life-time service, acrylic resin have weatherability it is good, protect
Light colour retention is excellent, heat-resist, there is certain decay resistance, and the acrylic resin of hydroxyl can with polyisocyanates reaction
The acroleic acid polyurethane film of prepared function admirable, it is of many uses, in order to reach double open coats for the requirement of low-surface-energy,
Acrylic acid fluorochemical monomer is introduced during synthesis of hydroxy acrylic resin, fluorine is introduced by perfluoroalkyl ethanol in isocyanate component
Element, resin system of the synthesis with low-surface-energy, and further increase the chemical-resistant of coating, anticorrosive property, resistance to
The cold performance such as heat-resisting, also hydrolyzes the silanol and silica particle surface in Ludox for producing using methyl tributanoximo silane
A part of hydroxyl there is intermolecular dehydration, add Methyl Hydrogen Polysiloxane Fluid, the silanol produced after hydrolysis and titanium dioxide silicon grain
The remaining hydroxyl in sublist face continues intermolecular dehydration, obtains modified hydrophobic Ludox, and using hydro-thermal reaction method
The load silver Graphene good stability of preparation, enables silver ion to be effectively deposited on surface of graphene oxide, effectively the group of preventing
It is poly-, good antibacterial effect is played, its surface is modified using hydrophobic sol, build the roughness in super-amphiphobic coating so as to from
Meet the requirement of double open coats in microstructure and surface composition on the whole, improve and easily disperse and antibiotic and sterilizing in coating
Deng effect, and good penetrability, the pore of substrate surface can be blocked, strengthen the adhesive force of coating, prepared by the present invention super
Double thin coating have good, heat-resisting, corrosion-resistant, the cold-resistant heat-resisting and anti-microbial property of non-adhesion behavior excellent, it is easy to the advantage of construction, coating
Adhesive force is high, difficult for drop-off, long service life, with higher actually used value.
Specific embodiment
A kind of super-amphiphobic silver system antibacterial composite hybridization corrosion resistant coating, by following weight portion（Kilogram）Raw material prepare system
Into：Perfluoroalkyl ethanol 32, methyl iso-butyl ketone (MIBK) 40, HDI trimer 90, methyl methacrylate 30, styrene 20, methyl-prop
Olefin(e) acid hydroxyl ethyl ester 8.5, the trifluoro monooctyl ester 17 of methacrylic acid ten, benzoyl peroxide 0.6, methanol Ludox 25, propylene glycol monomethyl ether
The ammonia of acetate 25,5% is appropriate, appropriate methyl tributanoximo silane, appropriate Methyl Hydrogen Polysiloxane Fluid, the fourth of 10% tin dilaurate two
Appropriate Ji Xi, dispersant 0.6, levelling agent 0.6, defoamer 0.4, appropriate butyl acetate, silver nitrate 2.3, graphene oxide 5.5,
Diallyldimethylammonium chloride 0.4, appropriate deionized water.
A kind of super-amphiphobic silver system antibacterial composite hybridization corrosion resistant coating, is made up of step in detail below：
（1）Perfluoroalkyl ethanol is mixed with the methyl iso-butyl ketone (MIBK) of butyl acetate, 2/3 times of amount, in being added to reaction bulb, starts to rise
Temperature is simultaneously slowly stirred to perfluoroalkyl ethanol and is completely dissolved, and instills the dibutyl tin laurates of 8 drops 10%, rises high-temperature to 70
After DEG C, the mixed liquor of Deca HDI trimer and butyl acetate, it is ensured that the completion of dropping in 1h is stepped up temperature to 90 DEG C, protects
Cooling down is standby as component A to room temperature after warm 2h；
（2）Appropriate butyl acetate is added to into vessel in heating to the insulation 20min that flows back, then by methyl methacrylate, benzene second
The mixing of alkene, hydroxyethyl methylacrylate, remaining methyl iso-butyl ketone (MIBK), 80% benzoyl peroxide and butyl acetate, wherein vinegar
Acid butyl ester is 3 with the volume ratio of methyl iso-butyl ketone (MIBK):1, the butyl acetate of above-mentioned backflow insulation is slowly dropped to after stirring and dissolving
In solution, it is ensured that completion of dropping in 1.5h, the trifluoro monooctyl ester of methacrylic acid ten is then rapidly added, rises high-temperature to 95 DEG C of backflows
Insulation 2h, is then disposably added to 10% benzoyl peroxide and appropriate butyl acetate mixing in container, insulation reaction 1h
Afterwards again by remaining benzoyl peroxide and the appropriate disposable addition of butyl acetate mixing, insulation reaction 1h is subsequently cooled to
50 DEG C, seal standby；
（3）Silver nitrate is added in deionized water the solution for making that concentration is 2wt%, in addition graphene oxide deionization is added to into
In water, ultrasonic disperse makes the dispersion liquid of 0.1wt%, then diallyldimethylammonium chloride ultrasonic agitation is added in dispersion liquid,
Stir and add silver nitrate solution in the backward mixed liquor, be placed in after stirring in hydrothermal reaction kettle, react at 160 DEG C
3h, is cooled to centrifugation after room temperature, and by product dehydrated alcohol and deionized water wash 3 times, is placed in baking oven after cleaning
Drying for standby at 90 DEG C；
（4）Methanol Ludox is placed in the container that bath temperature is 60 DEG C, total system quality is slowly added under agitation
Fraction is 12% methyl tributanoximo silane, and isothermal reaction 1h adds total system mass fraction for 3% Methyl Hydrogen Polysiloxane Fluid
Continue to react 1h, be subsequently adding after propylene glycol methyl ether acetate mix homogeneously and be transferred in rotary evaporator, vacuum distillation is removed
Methanol, obtains the scattered hydrophobically modified Ludox of propylene glycol methyl ether acetate；
（5）By step（3）The product of preparation is added to step（4）In, being placed in fully shaking in ultrasonator uniformly, then will be mixed
Compound is added to step（2）It is slowly stirred in the product of preparation to being uniformly dispersed, adds dispersant, levelling agent and defoamer at a high speed
Stirring 30min, rotating speed is controlled to 1000r/min, and then ultrasonic disperse 30min, then continues to high-speed stirred 20min, rotating speed control
700r/min is made as, component B is obtained, then by component A and component B according to mass ratio 1：3.2 mixing, room temperature is placed 10min and is entered
Row ripening, is adjusted to suitable viscosity with ethyl acetate and sprays or brush in surface of the work, and surface drying baking-curing at 80 DEG C is
Can.
Preparation method according to embodiment carries out performance test to its coating, as a result as follows：
Adhesive force:1 grade；Pliability：1mm；Hardness：5H；Impact strength：50mm；It it is 155-162 ° with the contact angle of deionized water；
It it is 152-155 ° with Oleum Arachidis hypogaeae semen contact angle；4 ° of roll angle ＜.
Claims (2)
1. a kind of super-amphiphobic silver system antibacterial composite hybridization corrosion resistant coating, it is characterised in that prepared by the raw material of following weight portion
Make：Perfluoroalkyl ethanol 32-35, methyl iso-butyl ketone (MIBK) 40-50, HDI trimer 90-100, methyl methacrylate 30-35,
Styrene 20-23, hydroxyethyl methylacrylate 8.5-9, the trifluoro monooctyl ester 17-19 of methacrylic acid ten, benzoyl peroxide 0.6-
0.8th, methanol Ludox 25-28, propylene glycol methyl ether acetate 25-26,5% ammonia is appropriate, methyl tributanoximo silane is fitted
Amount, appropriate Methyl Hydrogen Polysiloxane Fluid, 10% dibutyl tin laurate are appropriate, dispersant 0.6-1, levelling agent 0.6-0.8, defoamer
0.4-0.6, appropriate butyl acetate, silver nitrate 2.3-2.5, graphene oxide 5.5-6, diallyldimethylammonium chloride 0.4-
0.6th, appropriate deionized water.
2. a kind of super-amphiphobic silver system antibacterial composite hybridization corrosion resistant coating according to claim 1, it is characterised in that by following
Concrete steps are made：
（1）Perfluoroalkyl ethanol is mixed with the methyl iso-butyl ketone (MIBK) of butyl acetate, 2/3 times of amount, in being added to reaction bulb, starts to rise
Temperature is simultaneously slowly stirred to perfluoroalkyl ethanol and is completely dissolved, and instills the dibutyl tin laurate of 8-10 drops 10%, and liter high-temperature is extremely
After 70 DEG C, the mixed liquor of Deca HDI trimer and butyl acetate, it is ensured that the completion of dropping in 1h is stepped up temperature to 90 DEG C,
Cooling down is standby as component A to room temperature after insulation 2-3h；
（2）Appropriate butyl acetate is added to into vessel in heating to the insulation 20min that flows back, then by methyl methacrylate, benzene second
The mixing of alkene, hydroxyethyl methylacrylate, remaining methyl iso-butyl ketone (MIBK), 80% benzoyl peroxide and butyl acetate, wherein vinegar
Acid butyl ester is 3 with the volume ratio of methyl iso-butyl ketone (MIBK):1, the butyl acetate of above-mentioned backflow insulation is slowly dropped to after stirring and dissolving
In solution, it is ensured that completion of dropping in 1.5h, the trifluoro monooctyl ester of methacrylic acid ten is then rapidly added, rises high-temperature to 95 DEG C of backflows
Insulation 2h, is then disposably added to 10% benzoyl peroxide and appropriate butyl acetate mixing in container, insulation reaction 1-
After 1.5h remaining benzoyl peroxide and appropriate butyl acetate are mixed again and disposably added, insulation reaction 1-1.5h, with
After be cooled to 50 DEG C, seal standby；
（3）Silver nitrate is added in deionized water the solution for making that concentration is 2wt%, in addition graphene oxide deionization is added to into
In water, ultrasonic disperse makes the dispersion liquid of 0.1wt%, then diallyldimethylammonium chloride ultrasonic agitation is added in dispersion liquid,
Stir and add silver nitrate solution in the backward mixed liquor, be placed in after stirring in hydrothermal reaction kettle, at 160 DEG C 3- is reacted
4h, is cooled to centrifugation after room temperature, and by product dehydrated alcohol and deionized water wash 3 times, is placed in baking oven after cleaning
Drying for standby at 90 DEG C；
（4）Methanol Ludox is placed in the container that bath temperature is 60 DEG C, total system quality is slowly added under agitation
Fraction is 12% methyl tributanoximo silane, and isothermal reaction 1h adds total system mass fraction for 3% Methyl Hydrogen Polysiloxane Fluid
Continue to react 1h, be subsequently adding after propylene glycol methyl ether acetate mix homogeneously and be transferred in rotary evaporator, vacuum distillation is removed
Methanol, obtains the scattered hydrophobically modified Ludox of propylene glycol methyl ether acetate；
（5）By step（3）The product of preparation is added to step（4）In, being placed in fully shaking in ultrasonator uniformly, then will be mixed
Compound is added to step（2）It is slowly stirred in the product of preparation to being uniformly dispersed, adds dispersant, levelling agent and defoamer at a high speed
Stirring 30-50min, rotating speed is controlled to 1000-1200r/min, and then ultrasonic disperse 30-40min, then continues to high-speed stirred
20-30min, rotating speed is controlled to 700r/min, obtains component B, then by component A and component B according to mass ratio 1：3.2 mixing,
Room temperature is placed 10-15min and carries out ripening, is adjusted to suitable viscosity with ethyl acetate and is sprayed or brush after surface of the work, surface drying
The baking-curing at 80 DEG C.
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| CN201611143594.7A CN106634512A (en) | 2016-12-13 | 2016-12-13 | Super-amphiphobic silver series anti-microbial compound hybridizing anti-corrosion coating |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109181537A (en) * | 2018-07-16 | 2019-01-11 | 武汉疏能新材料有限公司 | A kind of super-amphiphobic SiO2The preparation method and application of nano functional liquid |
| CN110054756A (en) * | 2019-04-26 | 2019-07-26 | 同济大学 | The polyurethane resin and preparation method thereof of organic-silicon-modified fluorine-containing carbon branch |
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| CN110054756A (en) * | 2019-04-26 | 2019-07-26 | 同济大学 | The polyurethane resin and preparation method thereof of organic-silicon-modified fluorine-containing carbon branch |
| CN114292561A (en) * | 2021-12-06 | 2022-04-08 | 广东美涂士建材股份有限公司 | Organic silicon graphene industrial coating and preparation method thereof |
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