A kind of fluorine-containing superhydrophobic silicone coating compound and preparation method thereof

Abstract

The invention relates to the field of organic silicon compounds, aims to solve the defects that a conventional super-hydrophobic coating is poor in temperature and weather resistance, complex in preparation process, very thick in preparation concentration, has the super-hydrophobic property only in very low concentration, and the like, and discloses a fluorine-containing super-hydrophobic organic silicon coating compound and a preparation method thereof. The hardness of the organic silicon coating is 3H-6H after being cured for 3-48 hours at 10-40 DEG C, the water contact angle of the organic silicon coating is 150-165o, and the rolling angel of the organic silicon coating is smaller than 10o. The organic silicon coating is free of catalysts which can pollute the environment and can be produced in a large scale, and a product has the advantages of temperature and weather resistance, solvent corrosion resistance and the like of fluorine-containing organic silicon materials.

Description

technical field

[0001] The invention relates to the field of organosilicon composites, in particular to a superhydrophobic organosilicon coating and a preparation method thereof. Background technique

[0002] Superhydrophobic materials refer to materials with surface water contact angles greater than 150° and rolling angles less than 10°. They have broad application potential in the field of surface modification of windshields such as automobiles and aircraft, high-rise building wall glass, and glasses. Bravo et al [Langmuir, 2007,23 (13): 7293-7298] using fluorosilane modifier, SiO 2 Nanoparticles and sodium polystyrene sulfonate were self-assembled to prepare a transparent superhydrophobic coating with a water contact angle of 160°. Xu et al[J Mater Chem,2009,19:655-660] synthesized polystyrene microspheres by soap-free emulsion polymerization, and then combined the microspheres with inorganic SiO 2 Particle blending, ultrasonic vibration, and film coating, phase separat...

Examples

Embodiment 1

[0027] (1) React 205.28 g of 3-isocyanatopropyltrimethoxysilane with 82.05 g of difluoroethanol at 40°C for 24 hours to obtain 287.33 g of trifunctional fluorine-containing alkoxysilane;

[0028] (2) Add 80 g of deionized water and 1 g of acetic acid dropwise to the mixture of 100 g of trifunctional fluorine-containing alkoxysilane obtained in (1) and 5 g of toluene and 105 g of nano-silica, and complete the dropwise addition within 0.5 h. After reacting at 78°C for 4 hours, the layers were left to stand, the water phase was removed, and the toluene and residual water were removed under reduced pressure at 60°C / 20mmHg to obtain 68g of fluorine-containing silicone resin composite.

[0029] (3) Mix 68g of the fluorine-containing silicone resin compound obtained in (2), 68g of ethyl acetate, and 1.36g of isopropyl titanate evenly, seal it tightly, and store it at 30°C to obtain a fluorine-containing superhydrophobic silicone Coating Compound 1.

[0030] The fluorine-containing s...

Embodiment 2

[0032] (1) React 247 g of 3-isocyanatopropyltriethoxysilane with 100 g of trifluoroethanol at 30°C for 48 hours to obtain 347 g of trifunctional fluorine-containing alkoxysilane;

[0033] (2) Add 80 g of deionized water and 1 g of sulfuric acid to the mixture of 100 g of trifunctional fluorine-containing alkoxysilane, 15 g of nano-silicon dioxide, and 460 g of xylene obtained in (1), and complete the dropwise addition within 0.5 h , and reacted at 20°C for 24 h, stood to separate layers, removed the water phase, and removed xylene and residual water under reduced pressure at 140°C / 20mmHg to obtain 72 g of fluorine-containing silicone resin composite.

[0034] (3) Mix 72g of the fluorine-containing silicone resin compound obtained in (2), 36g of ethyl acetate, 108g of propylene glycol methyl ether acetate, and 10.8g of isopropyl titanate evenly, seal it, and store it at 25°C to obtain a A fluorine-containing superhydrophobic silicone coating compound 2.

[0035] The fluorine-c...

Embodiment 3

[0037] (1) React 205.28 g of 3-isocyanatopropyltrimethoxysilane with 132 g of tetrafluoropropanol at 40°C for 72 hours to obtain 337.28 g of trifunctional fluorine-containing alkoxysilane;

[0038] (2) Add 100 g of trifunctional fluorine-containing alkoxysilane, 1 g of nano-silica, and 31 g of ethyl acetate obtained in (1), dropwise a mixture of 100 g of deionized water and 5 g of p-toluenesulfonic acid, 0.5 The dropwise addition was completed within h, and after reacting at 40°C for 0.5 h, the layers were left to stand, the water phase was removed, and ethyl acetate and residual water were removed under reduced pressure at 100°C / 20mmHg to obtain the fluorine-containing silicone resin composite 52 g.

[0039](3) Mix 52 g of the fluorine-containing silicone resin compound obtained in (2), 520 g of ethyl acetate, and 1.36 g of the acetylacetone chelate of isopropyl titanate, mix evenly, seal it, and store it at 20°C to form a A fluorine-containing superhydrophobic silicone coat...

technical field

[0001] The invention relates to the field of organosilicon composites, in particular to a superhydrophobic organosilicon coating and a preparation method thereof. Background technique

[0002] Superhydrophobic materials refer to materials with surface water contact angles greater than 150° and rolling angles less than 10°. They have broad application potential in the field of surface modification of windshields such as automobiles and aircraft, high-rise building wall glass, and glasses. Bravo et al [Langmuir, 2007,23 (13): 7293-7298] using fluorosilane modifier, SiO 2 Nanoparticles and sodium polystyrene sulfonate were self-assembled to prepare a transparent superhydrophobic coating with a water contact angle of 160°. Xu et al[J Mater Chem,2009,19:655-660] synthesized polystyrene microspheres by soap-free emulsion polymerization, and then combined the microspheres with inorganic SiO 2 Particle blending, ultrasonic vibration, and film coating, phase separat...

Examples

Embodiment 1

[0027] (1) React 205.28 g of 3-isocyanatopropyltrimethoxysilane with 82.05 g of difluoroethanol at 40°C for 24 hours to obtain 287.33 g of trifunctional fluorine-containing alkoxysilane;

[0028] (2) Add 80 g of deionized water and 1 g of acetic acid dropwise to the mixture of 100 g of trifunctional fluorine-containing alkoxysilane obtained in (1) and 5 g of toluene and 105 g of nano-silica, and complete the dropwise addition within 0.5 h. After reacting at 78°C for 4 hours, the layers were left to stand, the water phase was removed, and the toluene and residual water were removed under reduced pressure at 60°C / 20mmHg to obtain 68g of fluorine-containing silicone resin composite.

[0029] (3) Mix 68g of the fluorine-containing silicone resin compound obtained in (2), 68g of ethyl acetate, and 1.36g of isopropyl titanate evenly, seal it tightly, and store it at 30°C to obtain a fluorine-containing superhydrophobic silicone Coating Compound 1.

[0030] The fluorine-containing s...

Embodiment 2

[0032] (1) React 247 g of 3-isocyanatopropyltriethoxysilane with 100 g of trifluoroethanol at 30°C for 48 hours to obtain 347 g of trifunctional fluorine-containing alkoxysilane;

[0033] (2) Add 80 g of deionized water and 1 g of sulfuric acid to the mixture of 100 g of trifunctional fluorine-containing alkoxysilane, 15 g of nano-silicon dioxide, and 460 g of xylene obtained in (1), and complete the dropwise addition within 0.5 h , and reacted at 20°C for 24 h, stood to separate layers, removed the water phase, and removed xylene and residual water under reduced pressure at 140°C / 20mmHg to obtain 72 g of fluorine-containing silicone resin composite.

[0034] (3) Mix 72g of the fluorine-containing silicone resin compound obtained in (2), 36g of ethyl acetate, 108g of propylene glycol methyl ether acetate, and 10.8g of isopropyl titanate evenly, seal it, and store it at 25°C to obtain a A fluorine-containing superhydrophobic silicone coating compound 2.

[0035] The fluorine-c...

Embodiment 3

[0037] (1) React 205.28 g of 3-isocyanatopropyltrimethoxysilane with 132 g of tetrafluoropropanol at 40°C for 72 hours to obtain 337.28 g of trifunctional fluorine-containing alkoxysilane;

[0038] (2) Add 100 g of trifunctional fluorine-containing alkoxysilane, 1 g of nano-silica, and 31 g of ethyl acetate obtained in (1), dropwise a mixture of 100 g of deionized water and 5 g of p-toluenesulfonic acid, 0.5 The dropwise addition was completed within h, and after reacting at 40°C for 0.5 h, the layers were left to stand, the water phase was removed, and ethyl acetate and residual water were removed under reduced pressure at 100°C / 20mmHg to obtain the fluorine-containing silicone resin composite 52 g.

[0039](3) Mix 52 g of the fluorine-containing silicone resin compound obtained in (2), 520 g of ethyl acetate, and 1.36 g of the acetylacetone chelate of isopropyl titanate, mix evenly, seal it, and store it at 20°C to form a A fluorine-containing superhydrophobic silicone coat...