CN101781506A - self-cleaning epoxy resin anti-fog coating - Google Patents
self-cleaning epoxy resin anti-fog coating Download PDFInfo
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Abstract
The invention belongs to the technical field of chemical materials, particularly relates to a self-cleaning epoxy resin anti-fog coating, which has high transparency and is composed of epoxide resin, firming agent, hydrophilic high polymer, surface active agent, functional nano particles and the like according to a proper proportion. The coating can be applied on the surfaces of glass, plastics and other base materials, and has excellent anti-fog and self-cleaning effects, good weather resistance and long service life.
Description
Technical field
The invention belongs to chemical material technical field, be specifically related to a kind of high-performance epoxy resin anti-fog coating.
Background technology
For a long time, transparent substrate has obtained using widely in people's production, life.Yet in the high environment for use of humidity, airborne water vapour is cohesion mist formation or dewdrop on these residuite surfaces easily, causes the transmittance of matrix to reduce, and hinders the use of base material.The infringement on attractive in appearance is not only in the influence that is brought, and even the people in production, the life are caused danger, easily cause traffic accident as the preformed casse on pilot lamp, car light, the glass for vehicle window.Past, simple mirror was antifog, normally add electricradiator at the back side of mirror and drive away illiteracy mist moisture, but this method has sizable limitation.Therefore, obtained people's extensive concern about the research of material with anti-fog performance.
Reports such as Zhang Chunxue have MMA, BMA, HEMA and little amount of crosslinking agent, N, and the coating that the polymerization of N-methylene radical diene acid amides constitutes has good anti-fog effect, but this antifog life-span of method gained coating is lacked [thermosetting resin 1999 (04): 28-30].Liu Guoxuan etc. are with methyl methacrylate, butyl methacrylate, acrylic acid copolymer, add a small amount of initiator and tensio-active agent (polyoxygenated alkane ether, alkyl benzene sulphonate (ABS) etc.) constitute anti-fog coating, but this method gained coating absorbs water not only anti-fog performance decline because of hydrophilic macromolecule, cause be full of cracks [Shanghai coating, 2005 (01): 31-33] simultaneously owing to swelling is softening.Nof Corp. is through exploring, earlier coat the organo-peroxide bottom at glass, resin, frosting, coating contains the high density polymer of hydrophilic radicals such as sulfonic group or hydroxyl again, form firm Chemical bond, realized the antifog New Machining Technology of semipermanent, but complete processing is very complicated, is unfavorable for industrialization promotion [JP 55-154351].Nissan Motor has reported that a kind of wetting ability films, coating one deck contains the laminated film of titanium dioxide and amorphous metal oxide on the outermost layer of matrix, because of containing the titanium dioxide of photocatalytic activity in filming, show to have Superhydrophilic by making after the illumination, and can decompose greasy dirt, have self-cleaning property, but this coating after long-term the placement, will lose its anti-fog performance [US 6071606] under the condition of darkroom or other shortage illumination.
Aforesaid method all has certain anti-fog effect, but deficiency is separately all arranged.。For this reason, exploitation is applicable to that simple and easy, the self-cleaning anti-fog coating of low cost, long lifetime, processing on the matrix such as glass, transparent resin has the staple market meaning.
Resins, epoxy is a kind of thermosetting resin, epoxy coating as main film forming material preparation, various metals, non-metal material surface and most filming all had good sticking power, help and the supporting use of the coating of other types, the chemical resistance of filming, physical strength, resistance toheat are superior, and the solidifying agent range of choice is wide, brought very big degree of freedom for prescription, the functional design of coating, it is very fine and close to film after solidifying simultaneously, can provide good performance for anti-fog coating.The hydrophilic macromolecule that is linked in the resin system can provide permanent anti-fog performance, the reaction surface promoting agent of hydrophilicity excellence can further promote anti-fog performance and be linked in the resin system and can not run off, function nano particle with photocatalysis performance can decompose the greasy dirt that remains in film coated surface under illumination, thereby realizes that self-cleaning performance also can improve, keep the antifog property of coating.
Summary of the invention
The purpose of this invention is to provide a kind of low cost, long lifetime, self-cleaning high-performance anti-fog coating.
Hydrophilic macromolecule anti-fog coating provided by the invention is made up of Resins, epoxy, hydrophilic high molecular material, solidifying agent, curing catalyst, tensio-active agent, functional nanomaterials, and the consumption of each component is as follows:
Resins, epoxy: 10-60wt%,
Hydrophilic macromolecule: 1-40wt%,
Solidifying agent: 1-40wt%,
Curing catalyst: 0.1-10wt%,
Reactive surfactant: 1-10wt%,
Functional nano particle: 0.1-10wt%,
Solvent: 30-80%wt,
Total amount satisfies 100%.
Except above component, also can add auxiliary agents such as an amount of flow agent, oxidation inhibitor according to conventional coating composition, at room temperature mix and can use.
Among the present invention, described Resins, epoxy is by being selected from: one or more of aliphatic glycidyl ether, aliphatic glycidyl ester, cycloaliphatic epoxy resin etc. are formed.Wherein, aliphatic glycidyl ether is as Polyethylene Glycol Bisglycidyl Ether, Racemic glycidol, polypropylene glycol glycidyl ether, propylene glycol diglycidylether, ethylene glycol diglycidylether etc.; The glycerol triglycidyl ether, trihydroxymethylpropanyltri diglycidyl ether etc.The aliphatic glycidyl ester is as hexahydrophthalic acid glycidyl ester, 1,2 epoxy cyclohexane 4,5-dioctyl phthalate glycidyl ester etc.; Cycloaliphatic epoxy resin is as vinyl cyclohexene dioxide, diformazan base band vinyl cyclohexene dioxide, bicyclopentadiene dioxide, titanium dioxide dicyclo amyl ether etc.The consumption of Resins, epoxy is: 10-60wt%, and wherein preferred: 15-50wt%, more preferably 15-40wt%.
Among the present invention, described solidifying agent is by being selected from: one or more of solidifying agent such as acid anhydrides, amine, cloudy release, resting form, light-initiated type are formed.The consumption of solidifying agent is: 0.1-40wt%, and wherein preferred: 0.2-30wt%, more preferably 0.2-20wt%.
Alicyclic, aliphatic anhydride class that acid anhydrides is mainly is as the adjacent phthalic anhydride of methyl six hydrogen, the adjacent phthalic anhydride of six hydrogen, poly-adipic anhydride, poly-nonane diacid acid anhydride, poly sebacic polyanhydride etc.; Amine curing agent is mainly aliphatic amide, polymeric amide, alicyclic and remodeling polyamine, as triethylene tetramine, isophorone diamine, N-amine ethyl piperazidine etc.; The anionic solidifying agent is mainly tertiary amines solidifying agent, imidazole curing agent class, as benzyldimethylamine, tetramethyl guanidine, glyoxal ethyline, 2-ethyl-4-methylimidazole, 2-undecyl imidazole, 2-heptadecyl imidazoles etc.; Latent curing agent is mainly Dyhard RU 100, boron trifluoride amine complex compound, as boron trifluoride mono aminoethane complex compound etc.; Light-initiated type solidifying agent is mainly diaryl iodine compound and triaryl matte compound, as: phenylbenzene iodine hexafluoro arsenate, triphenyl sulphur hexafluoro antimonate etc.
Among the present invention, described hydrophilic macromolecule is selected from: one or more of polyoxyethylene glycol and derivative thereof, polyoxyethylene glycol polypropylene glycol segmented copolymer, polyether glycol, polyester polyol, Polyvinylpyrolidone (PVP).The consumption of hydrophilic macromolecule is: 1-40wt%, wherein preferred 5-30wt%, more preferably 5-20wt%.
Among the present invention; described reactive surfactant is by being selected from: one or more formations of the tensio-active agent of hydroxyl, amino, carbon-carbon double bond or carboxyl,, empgen BB smooth as: polysorbate, lipid acid sorb, sodium dodecyl aminopropionitrile, 14 carbon-cetene base sodium sulfonate, sodium acryloyldimethyl taurate etc.The consumption of reactive surfactant is: 2-10wt%, and wherein preferred: 2-8wt%, more preferably 3-7wt%.
Among the present invention, described functional nano particle be selected from by: have the material of photocatalysis performance, as one or more compositions of nanoparticle of nanometer anatase titania, zinc oxide, Indium sesquioxide, zinc sulphide, indium hydroxide, gallium oxide etc.The consumption of functional nano particle is: 0.1-10wt%, and wherein preferred: 0.2-5wt%, more preferably 0.5-5wt%.
Anti-fog coating of the present invention can be selected general solvent for use, as ethylene glycol monomethyl ether, ethylene glycol monoethyl ether etc.By coating on base material, solidify, as the use of filming of antifog property.
As the generation type of filming of antifog property coating of the present invention, can adopt common spraying, roller coat, dipping Tu Fa etc., be not limited thereto, can adopt the method that is suitable for anti-fog coating of the present invention.
The curing mode of filming of anti-fog coating of the present invention has no particular limits, but uses the method that is heating and curing usually.Heating 30-180 minute or self-vulcanizing or irradiation 30-180 minute under the 365nm mercury lamp in adopting 50-150 ℃, the setting that solidification value and time can suit according to the reactivity of coating, the softening temperature of base material etc.
The thickness of filming of anti-fog coating of the present invention has no particular limits.The adjustment that can suit according to the performance of coating and base material.
Antifog principle of the present invention is to introduce hydrophilic macromolecule, reactive surfactant in resin coating, form super hydrophilic surface, its contact angle to water is diminished, do not form the small globule at surface spreading for moisture film as thin as a wafer, prevent that diffuse-reflectance from reaching antifogging action, and the activity of utilizing the photocatalytic nanometer particle decomposes greasy dirt and realizes its self-cleaning property under illumination, to improve, to keep the antifog property of coating.
Of the present invention filming done following test:
The film adhesive test is measured film adhesive according to the relevant clauses and subclauses of State Standard of the People's Republic of China GB1720-79 film adhesive assay method.Represent with level by the integrated degree evaluation of filming of far rolling in the cut scope.
The water-resistance property of coating test, the immersion laboratory method.It is in the distilled water of 40C that the sample that scribbles anti-fog coating is immersed temperature, observes once in per 24 hours, and record is filmed and begun to peel off or the corrugated time.
Anti-fog performance: a sample coatings face that scribbles anti-fog coating is placed the water tumbler top that 80C water is housed, and coating is apart from water surface 3cm, the mist formation time of visual inspection coating.
Above-mentioned test result all meets existing standard, and some indexs have exceeded existing standard, and it is low to prove absolutely that coating of the present invention has a cost, characteristics such as the life-span is long, anti-fog performance good, complete processing is simple.
Embodiment
Embodiment 1
Polyethylene Glycol Bisglycidyl Ether (400): 20g
Hexahydrophthalic anhydride: 10g
N, N-dimethyl benzylamine: 0.1g
Macrogol 4000: 8g
Polysorbate: 4g
Nano titanium oxide: 1g
Flow agent: 0.2g
Ethylene glycol monomethyl ether: 50g.
After stirring aforementioned coating composition all, spray to the surface of polycarbonate plate, in 100 ℃ of baking ovens, solidified 1 hour, so that paint solidification.
Embodiment 2
Bicyclopentadiene dioxide: 10g
Hexahydrophthalic anhydride: 18g
N, N-dimethyl benzylamine: 0.1g
Macrogol 4000: 8g
TX-6 nonionogenic tenside: 4g
Nano titanium oxide: 1g
Flow agent: 0.2g
Ethylene glycol monomethyl ether: 50g.
After stirring aforementioned coating composition all, spray to the surface of polycarbonate plate, in 100 ℃ of baking ovens, solidified 1 hour, so that paint solidification.
Embodiment 3
Hexahydrophthalic acid glycidyl ester: 15g
Hexahydrophthalic anhydride: 15g
N, N-dimethyl benzylamine: 0.1g
Macrogol 4000: 8g
Polysorbate: 4g
Nano titanium oxide: 1g
Flow agent: 0.2g
Ethylene glycol monomethyl ether: 50g.
After stirring aforementioned coating composition all, spray to the surface of polycarbonate plate, in 100 ℃ of baking ovens, solidified 1 hour, so that paint solidification.
Embodiment 4
Hexahydrophthalic acid glycidyl ester: 30g
Triethylene tetramine: 4g
Macrogol 4000: 8g
Empgen BB: 4g
Nano zine oxide: 1g
Flow agent: 0.2g
Ethylene glycol monoethyl ether: 50g.
After stirring aforementioned coating composition all, spray to the surface of polycarbonate plate, at room temperature solidify 1 day, so that paint solidification.
Embodiment 5
Hexahydrophthalic acid glycidyl ester: 30g
Dyhard RU 100: 2g
N, N-dimethyl benzylamine: 0.1g
Macrogol 4000: 8g
Empgen BB: 4g
Nano zine oxide: 1g
Flow agent: 0.2g
Ethylene glycol monoethyl ether: 50g.
After stirring aforementioned coating composition all, spray to the surface of polycarbonate plate, solidified 2 hours down at 100 ℃, so that paint solidification.
Embodiment 6
Polyethylene Glycol Bisglycidyl Ether (400): 30g
Boron trifluoride aniline complex compound: 0.5g
Polyethylene glycol 6000 monoleate: 8g
Sodium dodecyl aminopropionitrile: 4g
Nano titanium oxide: 1g
Flow agent: 0.2g
Ethylene glycol monobutyl ether: 50g.
After stirring aforementioned coating composition all, spray to the surface of polycarbonate plate, in 120 ℃ of baking ovens, solidified 1 hour, so that paint solidification.
Embodiment 7
Propylene glycol diglycidylether 30g
Phenylbenzene iodine hexafluoro arsenate: 0.5g
PEG/PPG segmented copolymer (50-HB-400): 8g
The lipid acid sorb is smooth: 4g
Nano oxidized gallium: 1g
Flow agent: 0.2g
Ethylene glycol monomethyl ether: 50g.
After stirring aforementioned coating composition all, spray to the surface of polycarbonate plate, irradiation was solidified 1 hour under the 365nm mercury lamp, so that paint solidification.
Embodiment 8
Polyethylene Glycol Bisglycidyl Ether (400): 20g
Hexahydrophthalic anhydride: 10g
N, N-dimethyl benzylamine: 0.1g
Polyvinylpyrolidone (PVP): 8g
The lipid acid sorb is smooth: 4g
Nano titanium oxide: 1g
Flow agent: 0.2g
Ethylene glycol monomethyl ether: 50g.
After stirring aforementioned coating composition all, spray to the surface of polycarbonate plate, in 100 ℃ of baking ovens, solidified 1 hour, so that paint solidification.
Embodiment 9
Polyethylene Glycol Bisglycidyl Ether (400): 30g
2-ethyl-4 Methylimidazole: 0.5g
Polyvinylpyrolidone (PVP): 8g
Sodium dodecyl aminopropionitrile: 4g
Nano titanium oxide: 1g
Flow agent: 0.2g
Ethylene glycol monobutyl ether: 50g.
After stirring aforementioned coating composition all, spray to the surface of polycarbonate plate, in 140 ℃ of baking ovens, solidified 2 hours, so that paint solidification.
Embodiment 10
Polyethylene Glycol Bisglycidyl Ether (400): 10g
Hexahydrophthalic acid glycidyl ester: 5g
Hexahydrophthalic anhydride: 10g
N, N-dimethyl benzylamine: 0.1g
Macrogol 4000: 8g
The lipid acid sorb is smooth: 4g
Nano titanium oxide: 1g
Flow agent: 0.2g
Ethylene glycol monomethyl ether: 50g.
After stirring aforementioned coating composition all, spray to the surface of polycarbonate plate, in 100 ℃ of baking ovens, solidified 1 hour, so that paint solidification.
The performance of table 1 embodiment coating
| Performance/numbering | ??1 | ??2 | ??3 | ??4 | ??5 |
| The transparency | Good | Good | Good | Good | Good |
| Sticking power | 1 grade | 1 grade | 1 grade | 1 grade | 1 grade |
| Water tolerance | ??180h | ??＞240h | ??＞240h | ??＞240h | ??＞??240h |
| Anti-fog effect | 56 seconds | 32 seconds | 40 seconds | 48 seconds | 44 seconds |
The performance of continuous table 1 embodiment coating
| Performance/numbering | ??6 | ??7 | ??8 | ??9 | ??10 |
| The transparency | Good | Good | Good | Good | Good |
| Sticking power | 1 grade | 1 grade | 1 grade | 1 grade | 1 grade |
| Performance/numbering | ??6 | ??7 | ??8 | ??9 | ??10 |
| Water tolerance | ??180h | ??120h | ??180h | ??＞240h | ??＞??240h |
| Anti-fog effect | ＞1 minute | 50 seconds | 50 seconds | 40 seconds | 54 seconds |
Show that after tested above-mentioned gained is filmed and all possessed anti-fog performance, film adhesive that different ingredients is formed and anti-mist performance be difference slightly, can satisfy under the different operating environment the antifog demand of material.
The above only is preferred embodiment of the present invention, is not to be that the present invention is done other forms of restriction, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the equivalent embodiment of equal variation.But every technical solution of the present invention content that do not break away to any simple modification, equivalent variations and remodeling that above embodiment did, still belongs to the protection domain of patented technology scheme of the present invention according to technical spirit of the present invention.
Claims (8)
1. a self-cleaning epoxy resin anti-fog coating is characterized in that being made up of Resins, epoxy, hydrophilic high molecular material, solidifying agent, curing catalyst, reactive surfactant, functional nanomaterials, and the consumption of each component is:
Resins, epoxy: 10-60wt%,
Hydrophilic macromolecule: 1-40wt%,
Solidifying agent: 1-40wt%,
Reactive surfactant: 1-10wt%,
Functional nano particle: 0.1-10wt%,
Solvent: 30-80%wt,
Total amount satisfies 100%.
2. anti-fog coating as claimed in claim 1 is characterized in that, described Resins, epoxy by: one or more in aliphatic glycidyl ether, aliphatic glycidyl ester, the cycloaliphatic epoxy resin are formed.
3. anti-fog coating as claimed in claim 1 is characterized in that, described solidifying agent is made up of in: acid anhydrides, amine, cloudy release, resting form, the light-initiated type solidifying agent one or more.
4. anti-fog coating as claimed in claim 3 is characterized in that, described acid anhydrides is alicyclic, aliphatic anhydride class;
Described amine curing agent is aliphatic amide, polymeric amide, alicyclic or remodeling polyamine;
Described anionic solidifying agent is tertiary amines solidifying agent or imidazole curing agent;
Described latent curing agent is boron trifluoride-amine complex or Dyhard RU 100;
Described light-initiated type solidifying agent is aromatic diazo salt, diaryl iodine compound or triaryl matte compound.
5. anti-fog coating as claimed in claim 1, it is characterized in that described hydrophilic macromolecule is by being selected from: one or more formations of polyoxyethylene glycol and derivative thereof, polyoxyethylene glycol polypropylene glycol segmented copolymer, polyethylene glycol stearate, polyester polyol, Polyvinylpyrolidone (PVP).
6. anti-fog coating as claimed in claim 1 is characterized in that, described reactive surfactant is by being selected from: one or more formations that contain the tensio-active agent of hydroxyl, amino, carbon-carbon double bond or carboxyl.
7. anti-fog coating as claimed in claim 1 is characterized in that, described functional nano particle is by being selected from: one or more form the nanoparticle of nanometer anatase titania, zinc oxide, Indium sesquioxide, zinc sulphide, indium hydroxide, gallium oxide.
8. anti-fog coating as claimed in claim 2 is characterized in that, described aliphatic glycidyl ether is: Polyethylene Glycol Bisglycidyl Ether, propylene glycol diglycidylether or trihydroxymethylpropanyltri diglycidyl ether; Described aliphatic glycidyl ester is: hexahydrophthalic acid glycidyl ester or 1,2 epoxy cyclohexane 4,5-dioctyl phthalate glycidyl ester; Described cycloaliphatic epoxy resin is: vinyl cyclohexene dioxide or diformazan base band vinyl cyclohexene dioxide.
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