CN102277060A - Hydrophobic ice-snow preventing coating material of fluorosilicone acrylate copolymer and preparation method of coating layer thereof - Google Patents
Hydrophobic ice-snow preventing coating material of fluorosilicone acrylate copolymer and preparation method of coating layer thereof Download PDFInfo
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Abstract
The invention discloses a hydrophobic ice-snow preventing coating material of a fluorosilicone acrylate copolymer and a preparation method of a coating layer thereof. The coating material comprises ethyl acetate serving as a solvent, and the solute of the solvent comprises a fluorosilicone acrylate copolymer and a solidifying agent. The preparation method of the coating layer by using the coating material comprises the following steps of: with an aluminum sheet as a substrate, cleaning the surface of the substrate by using acetone and water, and drying; and spraying the surface of the substrate at different distances from the surface of the substrate by using the coating material through a spray gun and air serving as power to obtain a super-hydrophobic coating layer with a micro-nano convex rough structure. According to the invention, the coating material has the advantages of simple coating material preparation process, easiness in obtaining the raw material, good formed film as well as good strength and hardness of the formed coating layer and can be widely used in surface coating of transportation, power transmission and other outdoor facilities; in addition; the preparation method of the coating layer has the advantages of simple process, no chemical processing, easiness for industrialization, suitability for large area applications, high practical value and excellent ice-snow preventing effect.
Description
Technical field
The present invention relates to a kind of hydrophobic anti-ice and snow coating and coating production of fluorine Si acrylate copolymer, belong to hydrophobic anti-ice and snow coating and applied technical field.
Background technology
Anti-icing is a global problem, and ice damage, the multiple country of snow disaster as countries and regions such as Canada, U.S. Northern Europe have been set up particular study mechanism already, carry out big quantity research to solving the icing problem.Usually adopt mechanical deicing at present both at home and abroad, be coated with and spread anti-icing agent, heating deicing and 4 kinds of de-icing methods of natural passive means deicing.Problems such as first three methods exists that working strength is big, efficient is low, contaminate environment, power consumption are big; Naturally passive deicing is by being coated with the coating of anti-icing at substrate surface, reducing ice to the sticking power of substrate surface and the ice cover on surface, utilizing wind and elemental effect to make ice break away from substrate surface easily again.These class methods are simple, cost is low, can play the effect that reduces ice damage in a lot of places.Therefore countries in the world all put forth effort to research and develop anti-icing paint (Gu Guangxin, military favorable to the people, for electricity consumption, 2008,3:35-37).
The application of hydrophobic coating in anti-icing field be a current wherein hot issue of research (R.Menini, M.Farzaneh, Journal of Adhesion Science and Technology, 2011,25:971-992).Organosilicon and fluorine material are two kinds of materials that known surface can be minimum in the nature all substances, so the fluorine Si acrylate copolymer is one of preferred material of preparation hydrophobic coating.The principle of the anti-icing of hydrophobic surface is based on the strong hydrophobicity performance of hydrophobic surface, and water droplet has lower cohesive force on its surface, be difficult in the surface accumulation, water droplet before freezing by self gravity or air outside power from surperficial landing.
The anti-icing hydrophobic coating of current research is most of to be adopted resin and nanoparticle etc. mineral filler is compound and be prepared from that (US 20100314575; M.Farzaneh, S.A.Kulinich, Applied Surface Science, 2011,257:6264-6269).Resin gives coating low surface energy, and nanoparticle gives coatingsurface certain roughness, thereby the two is in conjunction with making coating have superhydrophobic characteristic.Resin and nanoparticle dispersiveness are bad, nanoparticle needs hydrophobic treatment and causes problems such as complex process, cost increase but exist, and have influenced applying of super-hydrophobic coat to a certain extent.Can avoid the above-mentioned problem of mentioning and adopt polymkeric substance directly to prepare super-hydrophobic coat, existing at present multiple employing straight polymer prepares the technology of preparing of super hydrophobic surface, as plasma treatment technology (L.Jiang, H.Liu, L.Feng, D.Zhu, Langmuir, 2004,20:5659-5661), chemical vapour deposition (P.Favia, G.Cicala, A.Milella, F.Palumbo, R.Rossini, R.d ' Agostino, Surface and Coatings Technology, 2003,169:609-612) etc., but these technology preparation process complexity often need exacting terms or special plant and instrument, be not suitable for large-area film forming, also limited application.Song Yanlin (the He Min of the Chinese Academy of Sciences, Song Yanlin, ZL200810057287.6) and Li Xinxin seminar (Wei Haiyang, the Wang Kang of East China University of Science, the little reason of grain, Li Xinxin, Han Zhewen, polymer journal, 2008, (1): 69-75) adopt solvent film forming method to prepare the super hydrophobic surface of polymkeric substance respectively, the former needs drying under reduced pressure, and the used solvent of the latter is that Freon 113 (F-113) exerts an influence to atmospheric ozone layer.These two kinds of methods also are not suitable for large-area film forming.Adopt the application rarely seen report of the super-hydrophobic coat of straight polymer preparation in anti-icing field.
Summary of the invention
The object of the present invention is to provide a kind of hydrophobic anti-ice and snow coating and coating production of fluorine Si acrylate copolymer, this hydrophobic anti-ice and snow coating has superhydrophobic characteristic, and is easy to form uniform coating, and coating and ground tack are good, hardness is big, difficult drop-off, anti-ice and snow.
The present invention is realized by the following technical programs, a kind of hydrophobic anti-ice and snow coating of fluorine Si acrylate copolymer, it is characterized in that, this coating is under 20 ℃～60 ℃ in temperature, with ethyl acetate, butylacetate, acetone, butanone, wherein one or both of hexone and pimelinketone are solvent, contain quality and be 2%～30% solute in solvent, and described solute is for being 1 by fluorine Si acrylate copolymer and solidifying agent by mass ratio: 0.05-0.12 forms.
The structural formula of above-mentioned fluorine Si acrylate copolymer is shown in the formula 1, and its character is: the number-average molecular weight of multipolymer is: 8000～30000, and molecular weight distributing index is 1.5～2.8, mass loss is 5% o'clock heat decomposition temperature, T
d 5〉=400 ℃, after the multipolymer film forming to the contact angle of water greater than 110 °,
Formula 1
R
7For
R is alkyl or fluorinated alkyl in this structural unit.
Above-mentioned solidifying agent is selected from tolylene diisocyanate (TDI), 1, wherein one or both of 4-diphenylmethanediisocyanate (MDI), hexamethylene diisocyanate, hexamethylene diisocyanate oligopolymer (HDI) and isoflurane chalcone diisocyanate (IPDI).
Prepare the method for coating with the hydrophobic anti-ice and snow coating of above-mentioned fluorine Si acrylate copolymer, it is characterized in that comprising following process:
(1) be ground with aluminium flake, stainless steel substrates, copper sheet, iron plate, ceramic plate or sheet glass, clean its surface impurity and greasy dirt with acetone and water, and drying for standby;
(2) adopt the method preparation of aerial spraying to prevent the ice and snow hydrophobic coating, to the dry good substrate surface of step (1), adopting nozzle diameter is the spray gun of 0.2～5mm, with pressure is that 0.1～0.6MPa air is a power, apart from substrate surface 2～10cm place, the hydrophobic anti-ice and snow coating of fluorine Si acrylate copolymer is sprayed 3～5min to substrate surface, spray 3～5min again with distance substrate surface 15～50cm place then, after spraying finished, dry 5～72h promptly obtained having the super-hydrophobic coat of micro-nano protruding coarse structure under the room temperature.
The principle that the present invention adopts spraying method to prepare fluorine Si acrylate copolymer super-hydrophobic coat is: owing to there is the difference of solubleness between hydrophobic fluorine-containing groups or siloxanes segment and the hydrophilic segment in solvent, solvent effect multipolymer segmental in solution distributes and the gathering situation, also will have influence on the surface topography of film forming post polymerization thing film.The present invention adopts closely and the aerial spraying method that combines at a distance prepares fluorine Si acrylate copolymer super hydrophobic film.When closely spraying; solvent in the polymers soln has little time volatilization; " spheroidal particle " that polymkeric substance forms in solution bonds in the solvent evaporates process easily; merge mutually; the generation segmental is reset; inner hydroxyl is subjected to " inducing " of wetting ability ground in the multipolymer formed " spheroidal particle "; make hydrophilic segment to the strong ground migration of wetting ability; and hydrophobic fluorine-containing groups siloxanes segment moves to air surface; thereby at first formed whole smoother hydrophobic surface; when then adopting suitable remote spraying; solvent evaporates in the polymers soln is very fast, and the spheroidal particle of polymer formation can be bonded in smooth hydrophobic surface, the local fusion; make " spheroidal particle " firm being attached on the film surface of polymkeric substance, formed coarse super hydrophobic surface.
The principle of the anti-ice and snow of formed super-hydrophobic coat of the present invention is: utilized the ultra-hydrophobicity of coating, water droplet has very low adhesive power at coatingsurface, is difficult for accumulating at coatingsurface; Simultaneously, water droplet and super-hydrophobic coat surface contact area are very little, thermal conduction is slow, thereby prolonged the time that water droplet freezes, so, when water droplet does not also freeze, then lean on self gravity or air outside power, water droplet can not produce the snow phenomenon of freezing again then from the coatingsurface landing, has promptly reached anti-ice and snow effect.
The invention has the advantages that: the fluorine Si acrylate copolymer coating preparation process of the present invention's preparation is simple, raw material is easy to get, film forming is good, and the strength of coating and the hardness of formation are big, is widely used in outdoor facilities surfaces such as transport facility, oil drilling platform, power transmission and carries out coating.In the coating preparation process, processing method is simple, need not chemical treatment, need not exacting terms and special experimental installation, is easy to industrialization, is applicable to large-area application, has very high practical value, has good anti-ice and snow effect.
Description of drawings:
Fig. 1 is at room temperature being coated in hydrophobic coating that the aluminium flake surface the makes contact angle photo to water with the embodiment of the invention 1 obtained fluorine Si acrylate copolymer hydrophobic coating.
Fig. 2 is for being-10 ℃ of contact angle photos that are coated in hydrophobic coating that the aluminium flake surface makes to water with the embodiment of the invention 1 obtained fluorine Si acrylate copolymer hydrophobic coating in temperature.
By Fig. 1 and Fig. 2 as can be seen in room temperature to temperature-10 ℃ scope, prepared coating is constant substantially to the contact angle of water.
Fig. 3 is for to be coated in the stereoscan photograph that the aluminium flake surface makes the surface topography of hydrophobic coating with the embodiment of the invention 1 obtained fluorine Si acrylate copolymer hydrophobic coating.
Fig. 4 is under temperature-20 ℃, the water freezing photo that forms on the aluminium flake surface
Fig. 5 is for being coated in the coating that aluminium flake surface forms with the embodiment of the invention 1 obtained fluorine Si acrylate copolymer hydrophobic coating, the photo of water freezing does not take place under temperature-20 ℃.
Embodiment
Below by specific examples explanation the present invention, but the present invention is not only limited to these examples:
Embodiment 1
1) preparation of fluorine Si acrylate copolymer
Add hexone (10g) in reactor (250ml), logical nitrogen is heated to 70 ℃.With dripping by cyclohexyl methacrylate (12g), butyl acrylate (9g), hydroxyethyl methylacrylate (2g), reaching the solution that hexone (5g) is formed, drip the solution of being made up of hexone (5g) and Diisopropyl azodicarboxylate (0.3g) with another constant pressure funnel simultaneously, reaction is about 3 hours under this temperature.Slowly drip remaining Diisopropyl azodicarboxylate (0.15) and methacrylic acid ten difluoro heptyl esters (6g), 4-methacryloxy butyl-seven styryl POSS (1g) and remaining hexone (10g) then, 70 ℃ of reaction end in 24 hours down, cooling obtains translucent milkiness solution.Cool to 30 ℃, discharging is preserved.
2) preparation of coating
With above-mentioned synthetic fluorine Si acrylate copolymer (10g), the mixture that is dissolved in ethyl acetate (65g) and toluene (25g) under the room temperature is mixed with solution, and ultra-sonic oscillation after the dissolving, add TDI (0.5g), stir.
3) preparation of coating
Aluminium flake with 15cm * 10cm is a ground, cleans its surface impurity and greasy dirt, drying with acetone and water; Adopting nozzle diameter is the spray gun of 1mm, with pressure is that 0.1～0.2MPa air is a power, apart from aluminium flake surface 5 centimeters, the hydrophobic anti-ice and snow coating of the fluorine Si acrylate copolymer for preparing was sprayed 3 minutes to the aluminium flake surface, sprayed 5 minutes at room temperature dry 24 hours then then again with distance aluminium flake surface 30 centimeters.Performance to coating is tested, adopt JC2000D type contact angle measurement to record coating water contact angle is seen Fig. 1, super-hydrophobic coat is 157 ° to the contact angle of water under the room temperature, 4 ° of roll angles, when temperature is-10 °, contact angle to water is 152 ° of (see figure 2)s, and roll angle is 8 °, adopts Philips XL-30 type surface sweeping Electronic Speculum to record the coatingsurface pattern and sees Fig. 3.
4) anti-ice and snow experiment
Under-20 ℃ of environment, (15cm * 10cm) tilt 15 °, 300ml supercooled water that subsequently will-20 ℃ was poured on the aluminium flake that is coated with super-hydrophobic coat with 20 seconds time, repeated 3 times to make the aluminium flake that is coated with super-hydrophobic coat.Observe the icing situation of coatingsurface, and have the aluminium flake situation of freezing of super-hydrophobic coat to compare with uncoated.Experimental results show that to have good anti-ice and snow performance, do not freeze or only freeze on a small quantity, see Fig. 4 and Fig. 5 at the edge of coating at coatingsurface.
Embodiment 2
1) preparation of fluoro-acrylate copolymer
Add pimelinketone (9g) in reactor (250ml), logical nitrogen is heated to 80 ℃.With dripping by isobornyl acrylate (10g), octadecyl acrylate (10g), vinyltriethoxysilane (0.5g), reaching the solution that pimelinketone (5g) is formed, drip the solution of forming by pimelinketone (4g) and Diisopropyl azodicarboxylate (0.3g) with another constant pressure funnel simultaneously, reacted about 5 hours.Slowly drip remaining Diisopropyl azodicarboxylate (0.15) and methacrylic acid hexafluoro butyl ester (5g) and remaining pimelinketone (10g) then, react end in 4 hours, cooling obtains translucent milkiness solution.Cool to 30 ℃, discharging is preserved.
2) preparation of coating
With above-mentioned synthetic fluorine Si acrylate copolymer (30g), be dissolved in ethyl acetate (70g) under the room temperature and be mixed with solution, ultra-sonic oscillation after the dissolving, add MDI (2.4g), stir.
3) preparation of coating
Copper sheet with 15cm * 10cm is a ground, cleans its surface impurity and greasy dirt, drying with acetone and water; Adopting nozzle diameter is the spray gun of 2mm, with pressure is that 0.2～0.3MPa air is a power, apart from copper sheet surface 8 centimeters, the hydrophobic anti-ice and snow coating of the fluorine Si acrylate copolymer for preparing was sprayed 4 minutes to the copper sheet surface, sprayed 3 minutes at room temperature dry 36 hours then then again with distance copper sheet surface 20 centimeters.Performance to coating is tested, and adopts JC2000D type contact angle measurement to record coating to water contact angle, and super-hydrophobic coat is 155 ° to the contact angle of water under the room temperature, 5 ° of roll angles, when temperature is-10 °, be 152 ° to the contact angle of water, roll angle is 7 °.
4) anti-ice and snow experiment
Under-20 ℃ of environment, (15cm * 10cm) tilt 15 °, 300ml supercooled water that subsequently will-20 ℃ was poured on the stainless steel metal sheet that is coated with super-hydrophobic coat with 20 seconds time, repeated 3 times to make the copper sheet that is coated with super-hydrophobic coat.Observe the icing situation of coatingsurface, experimental results show that to have good anti-ice and snow performance, do not freeze or only freeze on a small quantity at the edge of coating at coatingsurface.
Embodiment 3
1) fluoro-acrylate copolymer is synthetic
Add toluene (12g) in reactor (250ml), logical nitrogen is heated to 110 ℃.With dripping by isobornyl methacrylate (10g), Octyl acrylate (10g), vinyl carbinol (2g), reaching the solution that toluene (6g) is formed, drip the solution of forming by toluene (4g) and dibenzoyl peroxide (0.3g) with another constant pressure funnel simultaneously, reacted about 3 hours.Slowly drip remaining dibenzoyl peroxide (0.15) and methacrylic acid ten trifluoro monooctyl esters (5g) and remaining toluene (10g) then, react end in 4 hours, cooling obtains translucent milkiness solution.Cool to 30 ℃, discharging is preserved.
2) preparation of coating
With above-mentioned synthetic fluorine Si acrylate copolymer (15g), be dissolved in acetone (85g) under the room temperature and be mixed with solution, ultra-sonic oscillation after the dissolving, add HDI (1.5g), stir.
The preparation of 30 coatings
Ceramic plate with 15cm * 10cm is a ground, cleans its surface impurity and greasy dirt, drying with acetone and water; Adopting nozzle diameter is the spray gun of 4mm, with pressure is that 0.4～0.5MPa air is a power, apart from ceramic plate surface 10 centimeters, the hydrophobic anti-ice and snow coating of the fluorine Si acrylate copolymer for preparing was sprayed 4 minutes to the ceramic plate surface, sprayed 5 minutes at room temperature dry 48 hours then then again with distance ceramic plate surface 40 centimeters.Performance to coating is tested, and adopts JC2000D type contact angle measurement to record coating to water contact angle, and super-hydrophobic coat is 159 ° to the contact angle of water under the room temperature, and 3 ° of roll angles in the time of-10 °, are 153 ° to the contact angle of water, 6 ° of roll angles.
4) anti-ice and snow experiment
Under-20 ℃ of environment, (15cm * 10cm) tilt 15 °, 300ml supercooled water that subsequently will-20 ℃ was poured on the ceramic plate that is coated with super-hydrophobic coat with 20 seconds time, repeated 3 times to make the ceramic plate that is coated with super-hydrophobic coat.Observe the icing situation of coatingsurface, experimental results show that to have good anti-ice and snow performance, do not freeze or only freeze on a small quantity at the edge of coating at coatingsurface.
Embodiment 4
1) fluoro-acrylate copolymer is synthetic
Add dimethylbenzene (6g) in reactor (250ml), logical nitrogen is heated to 85 ℃.With dripping by vinylbenzene (15g), methacrylic acid laurate (10g), Rocryl 410 (1.5g), reaching the solution that dimethylbenzene (9g) is formed, drip the solution of forming by toluene (4g) and Diisopropyl azodicarboxylate (0.3g) with another constant pressure funnel simultaneously, reacted about 3 hours.Slowly drip remaining Diisopropyl azodicarboxylate (0.15) and 4-methacryloxy butyl-seven styryl POSS (2g) and remaining dimethylbenzene (13g) then, react end in 48 hours, cooling obtains translucent milkiness solution.Cool to 30 ℃, discharging is preserved.
2) preparation of coating
With above-mentioned synthetic fluorine Si acrylate copolymer (20g), be dissolved in acetone (40g) under the room temperature and pimelinketone (40g) is mixed with solution, ultra-sonic oscillation after the dissolving, add HDI (1.2g), stir.
3) preparation of coating
Stainless steel substrates with 15cm * 10cm is a ground, cleans its surface impurity and greasy dirt, drying with acetone and water; Adopting nozzle diameter is the spray gun of 3mm, is power with pressure for the 0.3MPa air, apart from stainless steel substrates surface 5 centimeters, the hydrophobic anti-ice and snow coating of the fluorine Si acrylate copolymer for preparing was sprayed 1 minute to the stainless steel substrates surface, sprayed 5 minutes at room temperature dry 12 hours then then again with distance stainless steel substrates surface 50 centimeters.Performance to coating is tested, and adopts JC2000D type contact angle measurement to record coating to water contact angle, and super-hydrophobic coat is 155 ° to the contact angle of water under the room temperature, and 5 ° of roll angles in the time of-10 °, are 151 ° to the contact angle of water, 8 ° of roll angles.
4) anti-ice and snow experiment
Under-20 ℃ of environment, (15cm * 10cm) tilt 15 °, 300ml supercooled water that subsequently will-20 ℃ was poured on the stainless steel substrates that is coated with super-hydrophobic coat with 20 seconds time, repeated 3 times to make the stainless steel substrates that is coated with super-hydrophobic coat.Observe the icing situation of coatingsurface, experimental results show that to have good anti-ice and snow performance, do not freeze or only freeze on a small quantity at the edge of coating at coatingsurface.
Embodiment 5
1) preparation of coating
Fluorine Si acrylate copolymer (5g) and embodiment 4 synthetic fluorine Si acrylate copolymer (5g) of embodiment 2 is mixed, be dissolved in acetone (45g) under the room temperature and pimelinketone (45g) is mixed with solution, ultra-sonic oscillation are after the dissolving, add HDI (0.5g), stir.
2) preparation of coating
Sheet glass with 15cm * 10cm is a ground, cleans its surface impurity and greasy dirt, drying with acetone and water; Adopting nozzle diameter is the spray gun of 3mm, is power with pressure for the 0.3MPa air, apart from glass sheet surface 5 centimeters, the hydrophobic anti-ice and snow coating of the fluorine Si acrylate copolymer for preparing was sprayed 1 minute to glass sheet surface, sprayed 5 minutes at room temperature dry 12 hours then then again with distance glass sheet surface 50 centimeters.Performance to coating is tested, and adopts JC2000D type contact angle measurement to record coating to water contact angle, and super-hydrophobic coat is 155 ° to the contact angle of water under the room temperature, and 10 ° of roll angles in the time of-10 °, are 150 ° to the contact angle of water, 10 ° of roll angles.
3) anti-ice and snow experiment
Under-20 ℃ of environment, (15cm * 10cm) tilt 15 °, 300ml supercooled water that subsequently will-20 ℃ was poured on the sheet glass that is coated with super-hydrophobic coat with 20 seconds time, repeated 3 times to make the sheet glass that is coated with super-hydrophobic coat.Observe the icing situation of coatingsurface, experimental results show that to have good anti-ice and snow performance, do not freeze or only freeze on a small quantity at the edge of coating at coatingsurface.
Claims (4)
1. the hydrophobic anti-ice and snow coating of a fluorine Si acrylate copolymer, it is characterized in that, this coating is under 20 ℃～60 ℃ in temperature, with ethyl acetate, butylacetate, acetone, butanone, wherein one or both of hexone and pimelinketone are solvent, contain quality and be 2%～30% solute in solvent, described solute is for being 1: 0.05～0.12 to be made up of fluorine Si acrylate copolymer and solidifying agent by mass ratio.
2. press the hydrophobic anti-ice and snow coating of the described fluorine Si acrylate copolymer of claim 1, it is characterized in that, the structural formula of fluorine Si acrylate copolymer is shown in the formula 1, its character is: the number-average molecular weight of multipolymer is: 8000～30000, molecular weight distributing index is 1.5～2.8, mass loss is 5% o'clock heat decomposition temperature, T
d 5〉=400 ℃, after the multipolymer film forming to the contact angle of water greater than 110 °,
Formula 1
R
7For
R is alkyl or fluorinated alkyl in this structural unit.
3. press the hydrophobic anti-ice and snow coating of the described fluorine Si acrylate copolymer of claim 1, it is characterized in that, solidifying agent is selected from tolylene diisocyanate, 1, wherein one or both of 4-diphenylmethanediisocyanate, hexamethylene diisocyanate, hexamethylene diisocyanate oligopolymer and isoflurane chalcone diisocyanate.
4. one kind prepares the method for coating with the hydrophobic anti-ice and snow coating of the described fluorine Si acrylate copolymer of claim 1, it is characterized in that comprising following process:
(1) be ground with aluminium flake, stainless steel substrates, copper sheet, iron plate, ceramic plate or sheet glass, clean its surface impurity and greasy dirt with acetone and water, and drying for standby;
(2) adopt the method preparation of aerial spraying to prevent the ice and snow hydrophobic coating, to the dry good substrate surface of step (1), adopting nozzle diameter is the spray gun of 0.2～5mm, with pressure is that 0.1～0.6MPa air is a power, apart from substrate surface 2～10cm place, the hydrophobic anti-ice and snow coating of fluorine Si acrylate copolymer is sprayed 3～5min to substrate surface, spray 3～5min again with distance substrate surface 15～50cm place then, after spraying finished, dry 5～72h promptly obtained having the super-hydrophobic coat of micro-nano protruding coarse structure under the room temperature.
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