CN103013331A - Double-component fluorosilicone rubber ice-covering-proof coating material and preparation method thereof - Google Patents
Double-component fluorosilicone rubber ice-covering-proof coating material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a double-component fluorosilicone rubber ice-covering-proof coating material and a preparation method thereof. The preparation method comprises the following steps: dissolving fluorine-containing acrylate in solvent, adding a platinum catalyst, uniformly stirring, and pouring into a four-neck flask; starting an electromagnetic stirrer, introducing inert gas, heating in water bath, adding hydrogen-containing silicone oil, and reacting to generate fluorine modified silicone oil; placing vinyl terminated polydimethylsiloxane in a beaker, adding 5-40 parts by mass of white carbon black used as reinforcement filler, evenly stirring, then adding 0.5-5 parts by mass of whitener TiO2, and evenly stirring; weighing 1-5 parts by mass of hydrogen-containing silicone oil and 1-5 parts by mass of fluorine modified silicone oil, placing in the beaker, evenly stirring, adding 10-50mu L of platinum catalyst, and finally adding the solvent; and evenly coating through a spin coater, and curing in a baking oven for 1-4 hours, thus obtaining the double-component fluorosilicone rubber coating. The invention overcomes the defects in the prior art, uses polyorganosiloxane as the raw material, can achieve satisfactory ice-covering-proof effect and is used in the fields of paint and the like.
Description
Technical field
The invention belongs to the organic fluorinated silicone Material Field, more particularly, relate to a kind of pair of ice-covering-proof coated material of component trifluoropropyl siloxane and preparation method thereof.
Background technology
Accumulated snow or icing are long-pending at transmitting line, aircraft and other outdoor facility rich surfaces, easily cause transmitting line to fall the Serious Accidents such as bar (tower), broken string, air crash, produce incalculable damage.At present, develop the ice-covering-proof technology of kind more than 30, such as heat treating process, mechanical deicing's method, anti-icing paint method etc., but still do not solved ice-covering-proof problem fully.
In these ice-covering-proof technology, the anti-icing paint method is the most simple, and cost is low, and therefore, it more and more causes researchist's attention.At present, adoptable ice-covering-proof technology mainly is divided into two classes, initiatively deicing and passive anti-icing.Passive anti-icing be to adopt in easily the freeze method of position application low surface energy hydrophobic coating of aircraft to work.Passive anti-icing relative active deicing has that cost is low, power consumption is little, realize the characteristics such as difficulty is low, and can also reduce adhering to of ice, the generation that effectively is against any misfortune or alleviate the harm of freezing and may bring.
The material surface free energy is lower, and the adhesive attraction power of other materials and it is less, and concerning ice-covering-proof coating, that yes is more low better for surface free energy, and its surface free energy is lower, and ice body more is not easy to adhere to, and the ice body that perhaps adheres to is easier to come off.As everyone knows, the minimum material of surface energy of occurring in nature existence is fluorine material and organosilicon material.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, take organopolysiloxane as raw material, provide a kind of pair of ice-covering-proof coating of component trifluoropropyl siloxane and preparation method thereof.
Purpose of the present invention is achieved by following technical proposals:
A kind of pair of ice-covering-proof coated material of component trifluoropropyl siloxane and preparation method thereof, by the following method preparation:
(1) step 1 is got the fluorinated acrylate of 100 mass parts, is dissolved in the solvent, adds platinum catalyst, after stirring, under agitation condition, passes into rare gas element, adds containing hydrogen silicone oil and reacts generation fluorine modified silicon oil.
Wherein said platinum catalyst is ethylene methacrylic radical siloxane coordination platinum catalyst, and available from silicon mountain, Shanghai macromolecular material company, add-on is (3-21) * 10
-5Mass parts, preferred 15 * 10
-5Mass parts
Described rare gas element is nitrogen, helium or argon gas, preferred nitrogen.
Described solvent is dimethylbenzene, toluene or ethyl acetate, preferred dimethylbenzene.
Described fluorinated acrylate is vinylformic acid hexafluoro butyl ester, Hexafluorobutyl mathacrylate, methacrylic acid 2,2,2-trifluoro ethyl ester, dodecafluoroheptyl methacrylate, dodecafluorhe-ptylacrylate, methacrylic acid ten trifluoro monooctyl esters or vinylformic acid ten trifluoro monooctyl esters, preferred vinylformic acid hexafluoro butyl ester (G01 is available from the good fluorine chemistry of silicones of snow company limited).
Described stirring can be adopted mechanical stirring or induction stirring, and speed is that 30-80 turns/min.
Described temperature of reaction is 40-80 ℃, preferred 50-65 ℃, can be heated up and controls by heating in water bath; Reaction times is 5-30 hour, preferred 10-20 hour.
(2) step 2 is got the polydimethylsiloxane of the ethenyl blocking of 100 mass parts, adds 5-40 mass parts white carbon black as reinforced filling, and rear interpolation 0.5-5 mass parts whitening agent TiO stirs
2, stir
Described white carbon black is the modification fumed silica, and median size is 14 nanometers, preferred 10-15 mass parts.
Described whitening agent TiO2 median size is 21 nanometers, preferred 1 mass parts.
The polydimethylsiloxane viscosity of described ethenyl blocking is 2000-10000(25 ℃ of mPa.s), preferred 5000, available from the complete vertical chemical industry company limited of Wuxi City.
Described stirring can be adopted mechanical stirring or induction stirring, and speed is that 30-80 turns/min.
(3) step 3 adds 1-5 mass parts containing hydrogen silicone oil and 1-5 mass parts fluorine modified silicon oil in the system that stirs to step 2, rear adding (3-15) * 10 stirs
-5Mass parts platinum catalyst and solvent namely obtain two ice-covering-proof coated materials of component trifluoropropyl siloxane after stirring.
Described platinum catalyst is ethylene methacrylic radical siloxane coordination platinum catalyst, and available from silicon mountain, Shanghai macromolecular material company, consumption is preferably (4.5-7.5) * 10
-5Mass parts.
Described solvent is dimethylbenzene, toluene or ethyl acetate, preferred dimethylbenzene; Consumption is the 10-50 mass parts, preferred 20-40 mass parts.
Described stirring can be adopted mechanical stirring or induction stirring, and speed is that 30-80 turns/min.
Described fluorine modified silicon oil adopts the preparation method of step (1) to be prepared.
In technical scheme of the present invention, the containing hydrogen silicone oil that uses belongs to low-molecular-weight siloxanes, have the hydrogen that directly links to each other with Siliciumatom in the molecule, owing to contain the more active Si-H key of some amount in the molecule, under catalyst action, can react with other chemical substance that contains two strands, hydroxyl isoreactivity group, use the containing hydrogen silicone oil available from Jiangxi sea polyvoltine worker company limited, its hydrogen content (being the content of reactive hydrogen) is 0.75wt%.
In technical scheme steps of the present invention (1), in the fluorinated acrylate in the mole number of two keys and the containing hydrogen silicone oil ratio of the mole number of si-h bond (Si-H key) be (0.5-10): 1, preferably (2-8): 1.The mole number that when implementing, can calculate two keys in the fluorinated acrylate according to quality and the molar mass of the fluorinated acrylate that adds, as requested ratio is calculated the mole number of si-h bond again, owing to contain a reactive hydrogen in a si-h bond, the add-on of can be again calculating containing hydrogen silicone oil according to the hydrogen content of containing hydrogen silicone oil gets final product.
Infrared spectrum as shown in Figure 1,3470cm
-1The peak belong to the silicon W/O-the OH absorption peak; 2964cm
-1And 2905cm
-1The peak at place is-CH
3Vibration absorption peak, its checking peak position in 1470cm
-1The place; 2160cm
-1The place is the vibration absorption peak of Si-H in the containing hydrogen silicone oil; 1260cm
-1: peak shape is point by force, is the Si-CH in the siloxanes
3In-CH
3Symmetrical deformation vibration absorbs.The Si-O-Si group is at 1130～1000cm
-1Interior one or more very strong peaks that occurs.Accompanying drawing 2 is that several Fig. 2 are infrared spectrums of several hydrosilation products.Among the figure, 2160cm
-1The place is the vibration absorption peak of Si-H in the containing hydrogen silicone oil, and along with the increase of vinylformic acid hexafluoro butyl ester content, we can find out from spectrogram, 2160cm
-1The intensity of place's absorption peak reduces gradually, and this explanation is along with the increase of vinylformic acid hexafluoro butyl ester ratio, and the Si-H key reduces thereupon in the product, and namely the Si-H reaction is more complete in the containing hydrogen silicone oil.
After the two ice-covering-proof coated materials of component trifluoropropyl siloxane of preparation, can use sol evenning machine to smoothen at base material (glass or stainless steel metal), then 70-80 degree centigrade of lower curing at least 1 hour, preferably 1-4 hour, be more preferably 2-3 hour, namely get two component trifluoropropyl siloxane coatings.Technical scheme of the present invention adopts containing hydrogen silicone oil and fluorinated acrylate reaction, introduces fluorine element, generates two component fluorine silicon rubber coatings, easy to use to reach larger water contact angle and less this coating of ice shearing resistance, self-vulcanizing, environmental pollution is little, and the resource usage quantity is few.
Description of drawings
Fig. 1 is that the infrared spectrum of containing hydrogen silicone oil (adopts the U.S. Spectrum of Perkin-Elmer company 100 type Fourier transform infrared spectrometer, needs liquid sample 37 ℃ of freeze-day with constant temperature 24h in vacuum drying oven before analyzing; Spectral resolution: 0.5cm
-1, wavelength region: 4000～400cm
-1).
Fig. 2 is that the infrared spectrum of modification containing hydrogen silicone oil product among the embodiment 2-5 (adopts the U.S. Spectrum of Perkin-Elmer company 100 type Fourier transform infrared spectrometer, needs liquid sample 37 ℃ of freeze-day with constant temperature 24h in vacuum drying oven before analyzing; Spectral resolution: 0.5cm
-1, wavelength region: 4000～400cm
-1), wherein a is embodiment 2, and b is embodiment 3, and c is embodiment 4, and d is embodiment 5.
Embodiment
Further specify technical scheme of the present invention below in conjunction with specific embodiment.Platinum catalyst is ethylene methacrylic radical siloxane coordination platinum catalyst, available from silicon mountain, Shanghai macromolecular material company; The polydimethylsiloxane viscosity of ethenyl blocking is 2000-10000, and is preferred 5000, available from the complete vertical chemical industry company limited of Wuxi City; White carbon black is the modification fumed silica, and median size is 14 nanometers, whitening agent TiO
2Median size is 21 nanometers.Stirring in the implementation process can be adopted mechanical stirring or induction stirring, and speed is that 30-80 turns/min.
Embodiment 1
(1) step 1 is got 100g vinylformic acid hexafluoro butyl ester, is dissolved in the dimethylbenzene, adds 10 μ L platinum catalysts, after stirring, under agitation condition, pass into nitrogen, add containing hydrogen silicone oil and react and generate the fluorine modified silicon oil, temperature of reaction is 80 ℃, is heated up and controls by heating in water bath; Reaction times is 30 hours; In the vinylformic acid hexafluoro butyl ester in the mole number of two keys and the containing hydrogen silicone oil ratio of the mole number of si-h bond be 8:1.
(2) step 2 is got the polydimethylsiloxane of 100g ethenyl blocking, adds the 15g white carbon black as reinforced filling, and rear interpolation 5g whitening agent TiO stirs
2, stir
(3) step 3, add 5g containing hydrogen silicone oil and 5g in the system that stirs to step 2 through the fluorine modified silicon oil of step (1) preparation, stir rear adding 50 μ L platinum catalysts and 40g dimethylbenzene namely obtain two ice-covering-proof coated materials of component trifluoropropyl siloxane after stirring.
(4) step 4 uses sol evenning machine to smoothen in substrate of glass, then 80 degrees centigrade of lower curing 2 hours, namely gets two component trifluoropropyl siloxane coatings.
Embodiment 2
(1) step 1 is got 100g vinylformic acid hexafluoro butyl ester, is dissolved in the dimethylbenzene, adds 50 μ L platinum catalysts, after stirring, under agitation condition, pass into argon gas, add containing hydrogen silicone oil and react and generate the fluorine modified silicon oil, temperature of reaction is 65 ℃, is heated up and controls by heating in water bath; Reaction times is 20 hours; In the vinylformic acid hexafluoro butyl ester in the mole number of two keys and the containing hydrogen silicone oil ratio of the mole number of si-h bond be 0.5:1.
(2) step 2 is got the polydimethylsiloxane of 100g ethenyl blocking, adds the 10g white carbon black as reinforced filling, and rear interpolation 2g whitening agent TiO stirs
2, stir
(3) step 3, add 2g containing hydrogen silicone oil and 2g in the system that stirs to step 2 through the fluorine modified silicon oil of step (1) preparation, stir rear adding 25 μ L platinum catalysts and 50g dimethylbenzene namely obtain two ice-covering-proof coated materials of component trifluoropropyl siloxane after stirring.
(4) step 4 uses sol evenning machine to smoothen in substrate of glass, then 70 degrees centigrade of lower curing 3 hours, namely gets two component trifluoropropyl siloxane coatings.
Embodiment 3
(1) step 1 is got 100g vinylformic acid hexafluoro butyl ester, is dissolved in the dimethylbenzene, adds 30 μ L platinum catalysts, after stirring, under agitation condition, pass into helium, add containing hydrogen silicone oil and react and generate the fluorine modified silicon oil, temperature of reaction is 50 ℃, is heated up and controls by heating in water bath; Reaction times is 15 hours; In the vinylformic acid hexafluoro butyl ester in the mole number of two keys and the containing hydrogen silicone oil ratio of the mole number of si-h bond be 1:1.
(2) step 2 is got the polydimethylsiloxane of 100g ethenyl blocking, adds the 5g white carbon black as reinforced filling, and rear interpolation 0.5g whitening agent TiO stirs
2, stir
(3) step 3, add 1g containing hydrogen silicone oil and 1g in the system that stirs to step 2 through the fluorine modified silicon oil of step (1) preparation, stir rear adding 15 μ L platinum catalysts and 20g dimethylbenzene namely obtain two ice-covering-proof coated materials of component trifluoropropyl siloxane after stirring.
(4) step 4 uses sol evenning machine to smoothen in substrate of glass, then 80 degrees centigrade of lower curing 2 hours, namely gets two component trifluoropropyl siloxane coatings.
Embodiment 4
(1) step 1 is got 100g vinylformic acid hexafluoro butyl ester, is dissolved in the dimethylbenzene, adds 50 μ L platinum catalysts, after stirring, under agitation condition, pass into nitrogen, add containing hydrogen silicone oil and react and generate the fluorine modified silicon oil, temperature of reaction is 80 ℃, is heated up and controls by heating in water bath; Reaction times is 5 hours; In the vinylformic acid hexafluoro butyl ester in the mole number of two keys and the containing hydrogen silicone oil ratio of the mole number of si-h bond be 2:1.
(2) step 2 is got the polydimethylsiloxane of 100g ethenyl blocking, adds the 30g white carbon black as reinforced filling, and rear interpolation 2g whitening agent TiO stirs
2, stir
(3) step 3, add 2g containing hydrogen silicone oil and 4g in the system that stirs to step 2 through the fluorine modified silicon oil of step (1) preparation, stir rear adding 10 μ L platinum catalysts and 35g dimethylbenzene namely obtain two ice-covering-proof coated materials of component trifluoropropyl siloxane after stirring.
(4) step 4 uses sol evenning machine to smoothen in substrate of glass, then 70 degrees centigrade of lower curing 2 hours, namely gets two component trifluoropropyl siloxane coatings.
Embodiment 5
(1) step 1 is got 100g vinylformic acid hexafluoro butyl ester, is dissolved in the dimethylbenzene, adds 60 μ L platinum catalysts, after stirring, under agitation condition, pass into nitrogen, add containing hydrogen silicone oil and react and generate the fluorine modified silicon oil, temperature of reaction is 40 ℃, is heated up and controls by heating in water bath; Reaction times is 25 hours; In the vinylformic acid hexafluoro butyl ester in the mole number of two keys and the containing hydrogen silicone oil ratio of the mole number of si-h bond be 5.76:1.
(2) step 2 is got the polydimethylsiloxane of 100g ethenyl blocking, adds the 25g white carbon black as reinforced filling, and rear interpolation 2g whitening agent TiO stirs
2, stir
(3) step 3, add 2g containing hydrogen silicone oil and 2g in the system that stirs to step 2 through the fluorine modified silicon oil of step (1) preparation, stir rear adding 20 μ L platinum catalysts and 25g dimethylbenzene namely obtain two ice-covering-proof coated materials of component trifluoropropyl siloxane after stirring.
(4) step 4 uses sol evenning machine to smoothen in substrate of glass, then 70 degrees centigrade of lower curing 1 hour, namely gets two component trifluoropropyl siloxane coatings.
Embodiment 6
(1) step 1 is got 100g vinylformic acid hexafluoro butyl ester, is dissolved in the dimethylbenzene, adds 70 μ L platinum catalysts, after stirring, under agitation condition, pass into helium, add containing hydrogen silicone oil and react and generate the fluorine modified silicon oil, temperature of reaction is 50 ℃, is heated up and controls by heating in water bath; Reaction times is 10 hours; In the vinylformic acid hexafluoro butyl ester in the mole number of two keys and the containing hydrogen silicone oil ratio of the mole number of si-h bond be 10:1.
(2) step 2 is got the polydimethylsiloxane of 100g ethenyl blocking, adds the 40g white carbon black as reinforced filling, and rear interpolation 5g whitening agent TiO stirs
2, stir
(3) step 3, add 4g containing hydrogen silicone oil and 3g in the system that stirs to step 2 through the fluorine modified silicon oil of step (1) preparation, stir rear adding 15 μ L platinum catalysts and 10g dimethylbenzene namely obtain two ice-covering-proof coated materials of component trifluoropropyl siloxane after stirring.
(4) step 4 uses sol evenning machine to smoothen in substrate of glass, then 75 degrees centigrade of lower curing 1 hour, namely gets two component trifluoropropyl siloxane coatings.
After the two ice-covering-proof coated materials of component trifluoropropyl siloxane of preparation, can use sol evenning machine to smoothen in substrate of glass, then 70-80 degree centigrade of lower curing at least 1 hour, preferred 1-4 hour, be more preferably 2-3 hour, namely get two component trifluoropropyl siloxane coatings.In the use marine morning equipment company limited the static contact angle of JC2000D Static Contact angle measuring instrument measure sample under 25 degrees centigrade of room temperatures, the ice shearing resistance is according to the testing method of Cold Regions Research and Engineering Laboratory (CRREL) exploitation, use the incline high low temperature tension testing machine test of QJ211 (the Summer L.Sivas of skill Instr Ltd. of Shanghai, Bill Riegler, Rob Thomaier, Kelly Hoover, A Silicone-Based Ice-Phobic Coating for Aircraft, NuSil Technology LLC, Carpinteria, CA., U.S.Publisher:NuSil Technology LLC, Date:2007-11-08; Shuqing Yang, Qiang Xia, Lin Zhu et al.Research on the icephobic properties of fluoropolymer-based materials[J] .Applied Surface Science, 2011,257 (11): 4956-4962).
The contact angle of table 1 trifluoropropyl siloxane coating and ice shearing resistance
| Embodiment | Water contact angle (room temperature)/° | Ice shearing resistance/kPa |
| Embodiment 1 | 104.8 | 40.35 |
| Embodiment 2 | 105.9 | 22.28 |
| Embodiment 3 | 107.5 | 22.66 |
| Embodiment 4 | 111.3 | 32.08 |
| Embodiment 5 | 101.1 | 28.32 |
| Embodiment 6 | 103.5 | 35.24 |
The change fluorinated acrylate is Hexafluorobutyl mathacrylate, methacrylic acid 2,2,2-trifluoro ethyl ester, dodecafluoroheptyl methacrylate, dodecafluorhe-ptylacrylate, methacrylic acid ten trifluoro monooctyl esters or vinylformic acid ten trifluoro monooctyl esters; Changing solvent is toluene or ethyl acetate, also can realize technical scheme of the present invention and technique effect.
More than the present invention has been done exemplary description; should be noted that; in the situation that does not break away from core of the present invention, the replacement that is equal to that any simple distortion, modification or other those skilled in the art can not spend creative work all falls into protection scope of the present invention.
Claims (10)
1. two ice-covering-proof coated material of component trifluoropropyl siloxane is characterized in that, prepares by the following method:
(1) step 1, get the fluorinated acrylate of 100 mass parts, be dissolved in the solvent, add platinum catalyst, after stirring, under agitation condition, pass into rare gas element, add containing hydrogen silicone oil and react generation fluorine modified silicon oil, wherein said platinum catalyst is ethylene methacrylic radical siloxane coordination platinum catalyst, and add-on is (3-21) * 10
-5Mass parts; Described rare gas element is nitrogen, helium or argon gas; Described solvent is dimethylbenzene, toluene or ethyl acetate; Described fluorinated acrylate is vinylformic acid hexafluoro butyl ester, Hexafluorobutyl mathacrylate, methacrylic acid 2,2,2-trifluoro ethyl ester, dodecafluoroheptyl methacrylate, dodecafluorhe-ptylacrylate, methacrylic acid ten trifluoro monooctyl esters or vinylformic acid ten trifluoro monooctyl esters; Described stirring can be adopted mechanical stirring or induction stirring, and speed is that 30-80 turns/min; Described temperature of reaction is 40-80 ℃, can be heated up and controls by heating in water bath, and the reaction times is 5-30 hour; In the fluorinated acrylate in the mole number of two keys and the containing hydrogen silicone oil ratio of the mole number of si-h bond be (0.5-10): 1;
(2) step 2 is got the polydimethylsiloxane of the ethenyl blocking of 100 mass parts, adds 5-40 mass parts white carbon black as reinforced filling, and rear interpolation 0.5-5 mass parts whitening agent TiO stirs
2, stirring, the polydimethylsiloxane viscosity of wherein said ethenyl blocking is 2000-10000mPa.s, and described stirring can be adopted mechanical stirring or induction stirring, and speed is that 30-80 turns/min;
(3) step 3 adds 1-5 mass parts containing hydrogen silicone oil and 1-5 mass parts fluorine modified silicon oil in the system that stirs to step 2, rear adding (3-15) * 10 stirs
-5Mass parts platinum catalyst and solvent namely obtain two ice-covering-proof coated materials of component trifluoropropyl siloxane after stirring, wherein said platinum catalyst is ethylene methacrylic radical siloxane coordination platinum catalyst; Described solvent is dimethylbenzene, toluene or ethyl acetate, and consumption is the 10-50 mass parts; Described stirring can be adopted mechanical stirring or induction stirring, and speed is that 30-80 turns/min.
2. a kind of pair of ice-covering-proof coated material of component trifluoropropyl siloxane according to claim 1 is characterized in that, in the described step (1), and described platinum catalyst add-on preferred 15 * 10
-5Mass parts; Described rare gas element preferred nitrogen; The preferred dimethylbenzene of described solvent; The preferred vinylformic acid hexafluoro of described fluorinated acrylate butyl ester; The preferred 50-65 of described temperature of reaction ℃, can be heated up and controlled by heating in water bath; Preferred 10-20 of reaction times hour; The ratio preferred (2-8) of the mole number of si-h bond in the mole number of two keys and the containing hydrogen silicone oil in the described fluorinated monomer: 1.
3. a kind of pair of ice-covering-proof coated material of component trifluoropropyl siloxane according to claim 1 is characterized in that, in the described step (2), described white carbon black is the modification fumed silica, and median size is 14 nanometers, preferred 10-15 mass parts; Described whitening agent TiO2 median size is 21 nanometers, preferred 1 mass parts; The preferred 5000mPa.s of polydimethylsiloxane viscosity of described ethenyl blocking.
4. a kind of pair of ice-covering-proof coated material of component trifluoropropyl siloxane according to claim 1 is characterized in that, in the described step (3), described platinum catalyst is ethylene methacrylic radical siloxane coordination platinum catalyst, and consumption is preferably (4.5-7.5) * 10
-5Mass parts; The preferred dimethylbenzene of described solvent; The preferred 20-40 mass parts of consumption.
5. the preparation method of two ice-covering-proof coated materials of component trifluoropropyl siloxane is characterized in that, carries out according to following step:
(1) step 1, get the fluorinated acrylate of 100 mass parts, be dissolved in the solvent, add platinum catalyst, after stirring, under agitation condition, pass into rare gas element, add containing hydrogen silicone oil and react generation fluorine modified silicon oil, wherein said platinum catalyst is ethylene methacrylic radical siloxane coordination platinum catalyst, and add-on is (3-21) * 10
-5Mass parts; Described rare gas element is nitrogen, helium or argon gas; Described solvent is dimethylbenzene, toluene or ethyl acetate; Described fluorinated acrylate is vinylformic acid hexafluoro butyl ester, Hexafluorobutyl mathacrylate, methacrylic acid 2,2,2-trifluoro ethyl ester, dodecafluoroheptyl methacrylate, dodecafluorhe-ptylacrylate, methacrylic acid ten trifluoro monooctyl esters or vinylformic acid ten trifluoro monooctyl esters; Described stirring can be adopted mechanical stirring or induction stirring, and speed is that 30-80 turns/min; Described temperature of reaction is 40-80 ℃, can be heated up and controls by heating in water bath, and the reaction times is 5-30 hour; In the described acrylate in the mole number of two keys and the containing hydrogen silicone oil ratio of the mole number of si-h bond be (0.5-10): 1;
(2) step 2 is got the polydimethylsiloxane of the ethenyl blocking of 100 mass parts, adds 5-40 mass parts white carbon black as reinforced filling, and rear interpolation 0.5-5 mass parts whitening agent TiO stirs
2, stirring, the polydimethylsiloxane viscosity of wherein said ethenyl blocking is 2000-10000mPa.s, and described stirring can be adopted mechanical stirring or induction stirring, and speed is that 30-80 turns/min;
(3) step 3 adds 1-5 mass parts containing hydrogen silicone oil and 1-5 mass parts fluorine modified silicon oil in the system that stirs to step 2, rear adding (3-15) * 10 stirs
-5Mass parts platinum catalyst and solvent namely obtain two ice-covering-proof coated materials of component trifluoropropyl siloxane after stirring, wherein said platinum catalyst is ethylene methacrylic radical siloxane coordination platinum catalyst; Described solvent is dimethylbenzene, toluene or ethyl acetate, and consumption is the 10-50 mass parts; Described stirring can be adopted mechanical stirring or induction stirring, and speed is that 30-80 turns/min.
6. the preparation method of a kind of pair of ice-covering-proof coated material of component trifluoropropyl siloxane according to claim 5 is characterized in that, in the described step (1), and described platinum catalyst add-on preferred 15 * 10
-5Mass parts; Described rare gas element preferred nitrogen; The preferred dimethylbenzene of described solvent; The preferred vinylformic acid hexafluoro of described fluorinated acrylate butyl ester; The preferred 50-65 of described temperature of reaction ℃, can be heated up and controlled by heating in water bath; Preferred 10-20 of reaction times hour; The ratio preferred (2-8) of the mole number of si-h bond in the mole number of two keys and the containing hydrogen silicone oil in the described olefin(e) acid ester: 1.
7. the preparation method of a kind of pair of ice-covering-proof coated material of component trifluoropropyl siloxane according to claim 5 is characterized in that, in the described step (2), described white carbon black is the modification fumed silica, and median size is 14 nanometers, preferred 10-15 mass parts; Described whitening agent TiO2 median size is 21 nanometers, preferred 1 mass parts; The preferred 5000mPa.s of polydimethylsiloxane viscosity of described ethenyl blocking.
8. the preparation method of a kind of pair of ice-covering-proof coated material of component trifluoropropyl siloxane according to claim 5 is characterized in that, in the described step (3), described platinum catalyst is ethylene methacrylic radical siloxane coordination platinum catalyst, and consumption is preferably (4.5-7.5) * 10
-5Mass parts; The preferred dimethylbenzene of described solvent; The preferred 20-40 mass parts of consumption.
9. such as the using method of the described a kind of pair of ice-covering-proof coated material of component trifluoropropyl siloxane of one of claim 1-4, it is characterized in that, after the two ice-covering-proof coated materials of component trifluoropropyl siloxane of preparation, can use sol evenning machine to smoothen at base material, then 70-80 degree centigrade of lower curing at least 1 hour, namely get two component trifluoropropyl siloxane coatings.
10. the using method of a kind of pair of ice-covering-proof coated material of component trifluoropropyl siloxane according to claim 9 is characterized in that, preferred 1-4 hour 70-80 degree centigrade lower set time, is more preferably 2-3 hour.
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| CN103612460A (en) * | 2013-10-26 | 2014-03-05 | 溧阳市哈大成果转化中心有限公司 | Head leading edge assembly |
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| CN103625053A (en) * | 2013-10-26 | 2014-03-12 | 溧阳市哈大成果转化中心有限公司 | Front-edge component of anti-icing propeller blade |
| CN103625056A (en) * | 2013-10-30 | 2014-03-12 | 溧阳市哈大成果转化中心有限公司 | Front-edge component of engine air inlet duct of anti-icing aircraft |
| CN103625055A (en) * | 2013-10-30 | 2014-03-12 | 溧阳市哈大成果转化中心有限公司 | Coating-containing winglet leading edge |
| CN104263238A (en) * | 2014-09-11 | 2015-01-07 | 天津大学 | Fluoridated POSS (polysilsesquioxane) composite organic silicon coating as well as preparation method and anti-icing application thereof |
| CN105176391A (en) * | 2015-08-10 | 2015-12-23 | 湖南松井新材料有限公司 | Organosilicon coating |
| CN109852073A (en) * | 2018-08-30 | 2019-06-07 | 深圳市冠恒新材料科技有限公司 | Add-on type Fluorosilicone rubber composition and preparation method thereof, fluorine silicone rubber and coating |
| CN113527691A (en) * | 2021-06-24 | 2021-10-22 | 无锡龙驰氟硅新材料有限公司 | Fluorosilicone polymer and preparation method thereof |
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