CN102285177B - Organic anti-fog film - Google Patents
Organic anti-fog film Download PDFInfo
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- CN102285177B CN102285177B CN201110146708.4A CN201110146708A CN102285177B CN 102285177 B CN102285177 B CN 102285177B CN 201110146708 A CN201110146708 A CN 201110146708A CN 102285177 B CN102285177 B CN 102285177B
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- layer film
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Abstract
The invention relates to an organic anti-fog film, which adopts a double-layer film structure with the hydrophobic upper-layer film and the hydrophilic lower-layer film, a lower-layer film coated on the surface of a substrate consists of hydrophilic polymers or polymer molecules containing hydrophilic chain segments, an upper-layer film positioned on the surface of the lower-layer film consists of materials with low surface energy, the upper-layer film and the lower-layer film are combined through one kind of acting force or the combination of several kinds of acting force in Van der Waals force, hydrogen bond force, electrostatic force and covalence chemical bonds. Compared with the prior art, the anti-fog film disclosed by the invention has double effects of fog prevention and dirt prevention, the effect of fog prevention is lasting and effective, and the organic anti-fog film has no special requirements on the substrate, has a wide application scope and can be applied on the surfaces of various substrates such as glass, metal, ceramics and the like.
Description
Technical field
The present invention relates to the antifog technical field of matrix surface, particularly a kind of organic anti-fog film.
Background technology
In the middle of daily life, various matrixes such as glasses, glass for vehicle window, Restroom mirror, Discussion on architecture glass pane, agricultural greenhouse, place poor at high-temperature or that high humility is poor tends to occur knot mist and affects the use in life production, even can cause the loss of a large amount of manpowers and material resources.For example, when winter, wearing spectacles entered higher temperature indoor by lower temperature outdoor, on eyeglass, can inevitably produce one deck fog, impact is action normally; Equally, glass for vehicle window can be in humidity produces window mist in sombre or rainy season, affects driver driving; In addition, agricultural greenhouse tends to tie mist because of water evaporation in canopy, and the sunlight that affects canopy implants is taken in, thereby affects the normal growth of plant.
As can be seen here, the phenomenon of matrix surface knot mist brings tremendous influence can to daily life and production, and the antifog film of research matrix surface is the effective ways that address this problem, and has very important using value.
At present, mainly by two kinds of approach, obtain anti-fog performance: a kind of is based on hydrophobicity anti-fog method, and another kind is based on hydrophily anti-fog method.Hydrophobicity anti-fog method is to utilize water droplet larger at low-surface-energy Surface Contact, can leave surface by Free-rolling, thereby reach anti-fog effect, yet super hydrophobic surface obtains more difficult thereby develops less.Hydrophily anti-fog method is to utilize water very easily to sprawl to come at water-wetted surface to form transparent moisture film and play anti-fog effect.Particularly, building hydrophilic antifogging method has: 1) utilize surfactant method; 2) inorganic sol method; 3) hydrophilic macromolecule method; 4) TiO
2super-hydrophilic coating method.But hydrophily anti-fog method all suffers a fatal problem, water-wetted surface is easily by pollutions such as oil, dusts, and then loses anti-fog function, thereby need to spraying again after using certain hour, brings in actual use much inconvenience, in addition TiO
2super-hydrophilic coating need to be in competence exertion effect under illumination, thereby uses and restricted by environment.
Therefore, develop a kind of be not subject to environment for use restriction, can antipollution, have long-lasting, Novel fog-proof film is very significant cheaply.
Summary of the invention
The technical problem to be solved in the present invention is the deficiency for the above-mentioned state of the art, a kind of organic anti-fog film is provided, and this organic anti-fog film has advantages of good, the grease proofing and contamination by dust of anti-fog performance, surface light transmitance is high, adhesion is strong and applicable matrix scope is wide.
The present invention solves the problems of the technologies described above taked technical scheme: a kind of organic anti-fog film, adopt " parental type under upper dredging " double membrane structure, the lower membrane that is coated in matrix surface is to consist of hydrophilic polymer or the polymer molecule that contains hydrophilic segment, the upper layer film that is positioned at lower membrane surface is that the material by low-surface-energy forms, and between upper layer film and lower membrane, by a kind of active force in Van der Waals force, hydrogen bond force, electrostatic force and covalent chemical bond or the combination of several active forces, combines.
Described upper layer film is to consist of fluorine material or organosilicon material.Described fluorine material refers to some or all of replacement by fluorine atom of the hydrogen atom in organic molecule or polymer and the material that forms, and described organosilicon material refers to and contains R
1r
2r
3siO
1/2, R
1r
2siO or R
1siO
3/2the material of segment, wherein R
1, R
2, R
3be respectively C
6h
5-, C
nh
2n+1, C
mf
2m+1or C
mf
2m+1(CH
2)
n-, n is 0 to 20 integer, m is 1 to 20 integer.
Described fluorine material refers to and contains C
nf
2n+1, CF
3-(CF
2cF
2-CH
2cH
2)
n-, CF
3-(CF
2cH
2)
n-, CF
3-(C
2f
3c1)
n-, CF
3-(CF
2cF
2-CF
2cF (CF
3))
n-, CF
3-(CF
2cF (CF
3))
n, CF
3-(CF
2)
n(CH
2)
m-or
the organic molecule of unit or polymer, n wherein, m is the integer between 0 to 10000, preferably the integer between 1 to 100.
Described hydrophilic polymer has a kind of, two or more compositions or its polymer-modified formation in the polymer of better hydrophilicity including but not limited to polytetramethylene ether diol, polyethylene glycol, polypropylene glycol, polyvinyl alcohol, polyacrylic acid, polymethylacrylic acid, polyacrylamide and polyvinylpyrrolidone etc.For the worker of this area, hydrophilic polymer and add other polymer or hydrophilic polymer is carried out to modification in hydrophilic polymer, to improve hydrophilic polymer film-forming quality or adhesive property, be all well-known, these change the scope that does not exceed lower floor of the present invention hydrophilic membrane.
In order to improve the solvent resistance of coating, the molecular weight of preferred above-mentioned polytetramethylene ether diol is 600～50000, the molecular weight of polyethylene glycol is 200～60000, the molecular weight of polypropylene glycol is 400～25000, the molecular weight of polyvinyl alcohol is 1000～250000, polyacrylic molecular weight is 1000～50000, and the molecular weight of polymethylacrylic acid is 1000～50000, the molecular weight of polyacrylamide is 300～10000, the molecular weight of polyvinylpyrrolidone is 1000～700000.
Mentality of designing of the present invention is: organic anti-fog film is comprised of upper hydrophobic, lower hydrophilic double membrane structure, can play antifog and antifouling double effects simultaneously.The specific implementation of this mentality of designing is: lower floor's hydrophilic membrane is to consist of hydrophilic polymer or the polymer that contains hydrophilic segment, can improve water at this surperficial active force, reduce the surface contact angle of water, reach the surface wettability that improves water, thereby effective anti-sealing forms droplet on this surface, keep this surperficial light transmission performance, play antifouling fog effect; On this basis, increase the upper layer film with hydrophobic effect, this layer consists of the material of low-surface-energy, can effectively prevent oil, contamination by dust surface, keeps surface cleaning, makes whole antifog film anti-fog performance lasting for a long time.
Therefore, organic anti-fog film mentality of designing of the present invention is very ingenious, to those skilled in the art, hydrophily and hydrophobicity are the technology of knowing, the effect of these two technology is opposite each other, therefore those skilled in the art often thinks that hydrophilic antifogging, hydrophobic antifouling two technology can only realize separately, and the inventor's experience based on long-term research practice and thinking and produce inspiration just overcome this technology prejudice and completed the present invention.
In the time of in the environment of the matrix that applies organic anti-fog film of the present invention in easy knot mist, steam can condense at hydrophobic layer, yet due to interaction strong between water and hydrophilic layer, water droplet can be crossed hydrophobic layer by rapid permeability, and sprawl and come at hydrophilic layer, thereby play anti-fog effect; And the pollutants such as oil, dust cannot penetrate hydrophobic layer, anti-fouling effect can stop the pollution of pollutant to hydrophilic tunic, and then prevents that the function of antifog film is destroyed, and guarantees that hydrophilic antifogging film is effective lastingly.Be that antifog film involved in the present invention has overcome traditional hydrophily antifog film and subjects to a stained difficult problem.
Compared with prior art, the anti-fog performance of organic anti-fog film first of the present invention is splendid, owing to having double-decker design, reach antifog and antifouling double effects, thereby anti-fog effect is effective lastingly; Secondly, this organic anti-fog film does not have specific (special) requirements to matrix, for example, all have good adhesive force with the matrix of glass or other macromolecular materials formation, and wear-resisting and waterproof, thereby applied widely, can reach lasting weather-proof anti-fog performance; In addition, this organic anti-fog film has the simple and eco-friendly feature of production technology.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1:
A kind of organic anti-fog film of the present embodiment adopts " parental type under upper dredging " double-deck Molecular Design, the hydrophilic coating combination liquid that contains hydrophilic polymer is spin-coated on and treats that coat surface forms hydrophilic layer, then carbon tetrafluoride gas is processed and is combined in hydrophilic layer surface formation hydrophobic layer by low-temperature plasma, concrete steps are as follows:
Step 1: prepare hydrophilic coating combination liquid:
(1) 5 kilograms of acryloyl chlorides and 45 kilograms of cetomacrogol 1000s are added in reactor, at 90 ℃ of temperature, 2 hours acrylic acid synthesizing list macrogol esters of esterification under the protection of polymerization inhibitor, then be cooled to room temperature, decompression distillation desolventizes, and separated unreacted monomer, obtain hydrophilic acrylic resin's monomer;
(2) in temperature, be 50 ℃, under the effect of catalyst, acrylic acid list macrogol ester synthetic in (1) utilized to solution polymerization process polymerization 10 hours, synthetic HMW hydrophilic acrylic resin;
(3) (2) synthetic hydrophilic acrylic resin and 1 kilogram of toluene di-isocyanate(TDI) is well dispersed in 49 kilograms of ethyl acetate solvents, stirs, obtain hydrophilic coating combination liquid;
Step 2: the hydrophilic coating combination liquid that step 1 preparation is obtained is evenly coated on and treats coat surface formation hydrophilic coating by the method for spin coating;
Step 3: after hydrophilic coating completion of cure, be placed in low-temperature plasma processing instrument, pass into carbon tetrafluoride gas, maintenance vacuum is 20Pa, processes the fluorine-containing monolayer of one deck on hydrophilic coating surface, and the processing time is 8 minutes.
The organic anti-fog film of the matrix surface that above-mentioned preparation method obtains has splendid anti-fog performance, when water droplet drops on this antifog film, can rapid diffusion under the hydrophobic layer effect of upper strata, and then be penetrated into lower floor's hydrophilic layer, reduce knot mist, water droplet contact angle on this antifog film, only less than 30 °, can be sprawled rapidly because of water droplet, greatly avoids surface light transmitance to reduce; And the grease such as hexadecane contact angle on this antifogging surface is greater than 60 °, also there is certain antifouling effect on this surface; And this organic anti-fog film, to matrix is not had to specific (special) requirements, all has good adhesive force with the general matrix such as glass or other macromolecular materials formation, and wear-resisting and waterproof, can reach lasting weather-proof anti-fog performance; In addition, it is simple that this organic anti-fog film has production technology, and eco-friendly feature.
Embodiment 2:
A kind of organic anti-fog film of the present embodiment adopts " parental type under upper dredging " double-deck Molecular Design, the hydrophilic coating combination liquid that contains hydrophilic polymer is spin-coated on and treats that coat surface forms hydrophilic layer, then at these hydrophilic layer surface spin coating one deck ten trifluoro octyl group trimethoxy silane solution, by covalent bond, be combined with hydrophilic layer molecule, form stable hydrophobic layer, concrete steps are as follows:
Step 1, prepare hydrophilic coating combination liquid:
45 kilograms of Macrogol 200s and toluene di-isocyanate(TDI) are dispersed in acetone solvent, stir, then add 5 kilograms of ethyl orthosilicates, after stirring, obtain hydrophilic coating combination liquid;
Step 2: the hydrophilic coating combination liquid that step 1 preparation is obtained is evenly coated on and treats coat surface formation hydrophilic coating by the method for spin coating, and is heating and curing;
Step 3: after hydrophilic coating completion of cure, at surperficial spin coating one deck ten trifluoro octyl group trimethoxy silane solution, be combined with lower floor hydrophilic layer molecule by covalent bond, form and stablize upper strata oleophobic layer.
The organic anti-fog film of the matrix surface that above-mentioned preparation method obtains has splendid anti-fog performance, when water droplet drops on this antifog film, can rapid diffusion under the hydrophobic layer effect of upper strata, and then be penetrated into lower floor's hydrophilic layer, reduce knot mist, water droplet contact angle on this antifog film, only less than 20 °, can be sprawled rapidly because of water droplet, greatly avoids surface light transmitance to reduce; And the grease such as hexadecane contact angle on this antifogging surface is greater than 75 °, also there is certain antifouling effect on this surface; And this organic anti-fog film, to matrix is not had to specific (special) requirements, all has good adhesive force with the general matrix such as glass or other macromolecular materials formation, and wear-resisting and waterproof, can reach lasting weather-proof anti-fog performance; In addition, it is simple that this organic anti-fog film has production technology, and eco-friendly feature
Embodiment 3:
A kind of organic anti-fog film of the present embodiment adopts " parental type under upper dredging " double-deck Molecular Design, the hydrophilic coating combination liquid that contains hydrophilic polymer is spin-coated on and treats that coat surface forms hydrophilic layer, then at these hydrophilic layer surface spin coating one deck ten trifluoro octyl group trimethoxy silane solution, by covalent bond, be combined with hydrophilic layer molecule, form stable hydrophobic layer, concrete steps are as follows:
Step 1: prepare hydrophilic coating combination liquid:
(1) 6 kilograms of methacrylic chlorides and 42 kilograms of polytetramethylene ether diols 1000 are added in reactor, at 80 ℃ of temperature, 4 hours single polytetramethylene ether diol esters of synthesize methyl acrylic acid of esterification under the protection of polymerization inhibitor, then be cooled to room temperature, decompression distillation desolventizes, and separated unreacted monomer, obtain hydrophily methacrylic resin monomer;
(2) in temperature, be 120 ℃, under the effect of initator, methacrylic acid list macrogol ester synthetic in (1) utilized to solution polymerization process polymerization 8 hours, synthetic HMW hydrophilic acrylic resin;
(3) (2) synthetic hydrophilic acrylic resin and 2 kilograms of IPDIs are well dispersed in 50 kilograms of butyl acetate solvents, stir, obtain hydrophilic coating combination liquid;
Step 2: the hydrophilic coating combination liquid that step 1 preparation is obtained is evenly coated on and treats that coat surface forms hydrophilic coating by the method for being stained with painting;
Step 3: after hydrophilic coating completion of cure, be placed in low-temperature plasma processing instrument, pass into air gas, maintenance vacuum is 25Pa, hydrophilic coating surface enrichment great amount of hydroxy group after treatment, the processing time is 5 minutes.
Step 4: the mode of utilizing spin coating on the water-wetted surface of plasma treatment in step 3 preparation evenly applies one deck ten trifluoro octyl group trimethoxy silane solution, puts into baking oven and dries at 50 ° of temperature.
The organic anti-fog film of the matrix surface that above-mentioned preparation method obtains has splendid anti-fog performance, when water droplet drops on this antifog film, can rapid diffusion under the hydrophobic layer effect of upper strata, and then be penetrated into lower floor's hydrophilic layer, reduce knot mist, water droplet contact angle on this antifog film, only less than 25 °, can be sprawled rapidly because of water droplet, greatly avoids surface light transmitance to reduce; And the grease such as hexadecane contact angle on this antifogging surface is greater than 70 °, also there is certain antifouling effect on this surface; And this organic anti-fog film, to matrix is not had to specific (special) requirements, all has good adhesive force with the general matrix such as glass or other macromolecular materials formation, and wear-resisting and waterproof, can reach lasting weather-proof anti-fog performance; In addition, it is simple that this organic anti-fog film has production technology, and eco-friendly feature.
Embodiment 4:
A kind of organic anti-fog film of the present embodiment adopts " parental type under upper dredging " double-deck Molecular Design, the hydrophilic coating combination liquid that contains hydrophilic polymer is spin-coated on and treats that coat surface forms hydrophilic layer, then at this hydrophilic layer surface spin coating one deck perfluor quaternary cationics solution, by covalent bond, be combined with lower floor hydrophilic layer molecule, form stable upper strata hydrophobic layer, concrete steps are as follows:
Step 1: prepare hydrophilic coating combination liquid:
45 kg polypropylene acid are fully dissolved in acetone solvent, stir, then add 5 kilograms of positive silicic acid second
Ester, obtains hydrophilic coating combination liquid;
Step 2: the hydrophilic coating combination liquid that step 1 preparation is obtained is evenly coated on and treats coat surface formation hydrophilic coating by the method for spin coating, and is heating and curing;
Step 3: after hydrophilic coating completion of cure, at surperficial spin coating one deck perfluor quaternary cationics solution, be combined with lower floor hydrophilic layer molecule by electrostatic force bonding, form stable upper strata hydrophobic layer.
The organic anti-fog film of the matrix surface that above-mentioned preparation method obtains has splendid anti-fog performance, when water droplet drops on this antifog film, can rapid diffusion under the hydrophobic layer effect of upper strata, and then be penetrated into lower floor's hydrophilic layer, reduce knot mist, water droplet contact angle on this antifog film, only less than 30 °, can be sprawled rapidly because of water droplet, greatly avoids surface light transmitance to reduce; And the grease such as hexadecane contact angle on this antifogging surface is greater than 65 °, also there is certain antifouling effect on this surface; And this organic anti-fog film, to matrix is not had to specific (special) requirements, all has good adhesive force with the general matrix such as glass or other macromolecular materials formation, and wear-resisting and waterproof, can reach lasting weather-proof anti-fog performance; In addition, it is simple that this organic anti-fog film has production technology, and eco-friendly feature.
Claims (4)
1. an organic anti-fog film, it is characterized in that: described organic anti-fog film is comprised of upper and lower two membranes, the lower membrane that is coated in matrix surface is to consist of hydrophilic polymer or the polymer molecule that contains hydrophilic segment, and the upper layer film that is positioned at lower membrane surface is that the material by low-surface-energy forms
Between upper layer film and lower membrane, by a kind of active force in Van der Waals force, hydrogen bond force, electrostatic force and covalent chemical bond or the combination of several active forces, combine;
In the time of in the environment of the matrix that applies described organic anti-fog film in easy knot mist, steam will condense at upper layer film, and water droplet is by infiltration upper layer film and sprawl and come in lower membrane, and oily, dust cannot permeate upper layer film;
Described hydrophilic polymer is a kind of, two or more composition in polytetramethylene ether diol, polyethylene glycol, polypropylene glycol, polyvinyl alcohol, polyacrylic acid, polymethylacrylic acid, polyacrylamide and polyvinylpyrrolidone or it is polymer-modified;
Described upper layer film is to consist of fluorine material or organosilicon material;
Described fluorine material refers to that the hydrogen atom in organic molecule or polymer is some or all of by material that fluorine atom replaced;
Described organosilicon material refers to and contains R
1r
2r
3siO
1/2, R
1r
2siO or R
1siO
3/2the material of segment, wherein R
1, R
2, R
3be respectively C
6h
5-, C
nh
2n+1, C
mf
2m+1or C
mf
2m+1(CH
2)
n-, n is 0 to 20 integer, m is 1 to 20 integer.
2. organic anti-fog film according to claim 1, is characterized in that: described fluorine material refers to and contains C
nf
2n+1, CF
3-(CF
2cF
2-CH
2cH2)
n-, CF
3-(CF
2cH
2)
n-, CF
3-(C
2f
3cl)
n-,
CF
3-(CF
2cF
2-CF
2cF (CF
3))
n-, CF
3-(CF
2cF (CF
3))
n, CF
3-(CF
2)
n(CH
2)
m-or
the organic molecule of unit or polymer, n wherein, m is the integer between 0 to 10000.
3. organic anti-fog film according to claim 2, is characterized in that: described n, m is the integer between 1 to 100.
4. organic anti-fog film according to claim 1, it is characterized in that: the molecular weight of described polytetramethylene ether diol is 600～50000, the molecular weight of polyethylene glycol is 200～60000, the molecular weight of polypropylene glycol is 400～25000, the molecular weight of polyvinyl alcohol is 1000～250000, polyacrylic molecular weight is 1000～50000, and the molecular weight of polymethylacrylic acid is 1000～50000, the molecular weight of polyacrylamide is 300～10000, the molecular weight of polyvinylpyrrolidone is 1000～700000.
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|---|---|---|---|
| CN201110146708.4A CN102285177B (en) | 2011-06-01 | 2011-06-01 | Organic anti-fog film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110146708.4A CN102285177B (en) | 2011-06-01 | 2011-06-01 | Organic anti-fog film |
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| CN102285177A CN102285177A (en) | 2011-12-21 |
| CN102285177B true CN102285177B (en) | 2014-09-03 |
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ID=45332034
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| CN103818082A (en) * | 2013-12-31 | 2014-05-28 | 保定宝理塑研包装有限公司 | Coating type multifunctional long-lasting mirror surface sunlight greenhouse membrane and production method thereof |
| CN106976291B (en) * | 2017-03-29 | 2019-02-19 | 嘉兴市南湖花卉园艺工程有限公司 | A kind of awning film and preparation method thereof |
| CN111330824B (en) * | 2020-03-24 | 2022-10-04 | 佛山市思博睿科技有限公司 | Organic plate surface plasma super-hydrophilic nano anti-fog treatment method and application |
| CN113787799A (en) * | 2021-09-03 | 2021-12-14 | 富维薄膜（山东）有限公司 | Novel water mist-proof film and preparation method thereof |
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| JP4887622B2 (en) * | 2004-12-17 | 2012-02-29 | セントラル硝子株式会社 | Antifogging article, method for producing the same, and coating agent for forming antifogging film |
| CN1303137C (en) * | 2005-04-19 | 2007-03-07 | 华东理工大学 | Exterior coating antifogging film and preparation method |
| JP5332205B2 (en) * | 2005-11-01 | 2013-11-06 | 旭硝子株式会社 | Antifogging article and antifogging agent composition |
| JP5234451B2 (en) * | 2007-10-03 | 2013-07-10 | 山本光学株式会社 | Double lens |
| CN101709194A (en) * | 2009-11-27 | 2010-05-19 | 上海理工大学 | Antifog spray coating material and applications thereof |
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