Fluorine-containing super-hydrophobic organic silicon 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 super-hydrophobic organosilicon coating and a preparation method thereof. Background technique

[0002] Superhydrophobic materials refer to materials whose surface water contact angle is greater than 150° and rolling angle is less than 10°. Bravo et al [Langmuir, 2007, 23 (13): 7293-7298] used fluorosilane modifier, SiO 2 A transparent superhydrophobic coating with a water contact angle of 160° was prepared by self-assembly of nanoparticles and sodium polystyrene sulfonate. Xu et al [J Mater Chem, 2009, 19:655-660] synthesized polystyrene microspheres by soap-free emulsion polymerization, and then mixed the microspheres with inorganic SiO 2 Particle blending, coating after ultrasonic oscillation, phase separation at a high temperature of 500 ℃ and obtaining a crater-like microstructure, after surface modification with fluorosilane coupling agent, the visible light tran...

Examples

Embodiment 1

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

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

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

[003...

Embodiment 2

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

[0033] (2) To the mixture of 100 g of trifunctional fluorine-containing alkoxysilane, 15 g of nano-silica, and 460 g of xylene obtained in (1), add dropwise a mixture of 80 g of deionized water and 1 g of sulfuric acid, and the dropwise addition is completed within 0.5 h , and reacted at 20 °C for 24 h, left to stand for stratification, removed the aqueous phase, and removed xylene and residual water under reduced pressure at 140 °C / 20 mmHg to obtain 72 g of a fluorine-containing silicone resin composite.

[0034] (3) Mix 72 g of the fluorine-containing silicone resin compound obtained in (2), 36 g of ethyl acetate, 108 g of propylene glycol methyl ether acetate, and 10.8 g of isopropyl titanate. A fluorine-containing superhydrophobic silicone coating composite 2.

[0035] The fluorine-containin...

Embodiment 3

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

[0038] (2) To the mixture of 100 g of trifunctional fluorine-containing alkoxysilane, 1 g of nano-silica, and 31 g of ethyl acetate obtained in (1), add dropwise a mixture of 100 g of deionized water and 5 g of p-toluenesulfonic acid, 0.5 g The dropwise addition was completed within h, and after reacting at 40 °C for 0.5 h, the layers were left standing to remove the aqueous phase, and the ethyl acetate and residual water were removed under reduced pressure at 100 °C / 20 mmHg to obtain a 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 evenly, seal it, and store it at 20 °C, which is a A fluorine-containing super...

technical field

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

[0002] Superhydrophobic materials refer to materials whose surface water contact angle is greater than 150° and rolling angle is less than 10°. Bravo et al [Langmuir, 2007, 23 (13): 7293-7298] used fluorosilane modifier, SiO 2 A transparent superhydrophobic coating with a water contact angle of 160° was prepared by self-assembly of nanoparticles and sodium polystyrene sulfonate. Xu et al [J Mater Chem, 2009, 19:655-660] synthesized polystyrene microspheres by soap-free emulsion polymerization, and then mixed the microspheres with inorganic SiO 2 Particle blending, coating after ultrasonic oscillation, phase separation at a high temperature of 500 ℃ and obtaining a crater-like microstructure, after surface modification with fluorosilane coupling agent, the visible light tran...

Examples

Embodiment 1

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

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

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

[003...

Embodiment 2

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

[0033] (2) To the mixture of 100 g of trifunctional fluorine-containing alkoxysilane, 15 g of nano-silica, and 460 g of xylene obtained in (1), add dropwise a mixture of 80 g of deionized water and 1 g of sulfuric acid, and the dropwise addition is completed within 0.5 h , and reacted at 20 °C for 24 h, left to stand for stratification, removed the aqueous phase, and removed xylene and residual water under reduced pressure at 140 °C / 20 mmHg to obtain 72 g of a fluorine-containing silicone resin composite.

[0034] (3) Mix 72 g of the fluorine-containing silicone resin compound obtained in (2), 36 g of ethyl acetate, 108 g of propylene glycol methyl ether acetate, and 10.8 g of isopropyl titanate. A fluorine-containing superhydrophobic silicone coating composite 2.

[0035] The fluorine-containin...

Embodiment 3

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

[0038] (2) To the mixture of 100 g of trifunctional fluorine-containing alkoxysilane, 1 g of nano-silica, and 31 g of ethyl acetate obtained in (1), add dropwise a mixture of 100 g of deionized water and 5 g of p-toluenesulfonic acid, 0.5 g The dropwise addition was completed within h, and after reacting at 40 °C for 0.5 h, the layers were left standing to remove the aqueous phase, and the ethyl acetate and residual water were removed under reduced pressure at 100 °C / 20 mmHg to obtain a 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 evenly, seal it, and store it at 20 °C, which is a A fluorine-containing super...