Preparation method and application of solvent-type hydrophobic and oleophobic fluoroalkyl silicone resin

The technology of fluorocarbon-based silicone resin and fluorocarbon-based halosilane is applied in the preparation field of solvent-based hydrophobic and oleophobic fluorocarbon-based silicone resin, which can solve the problems of complicated steps and the like, and achieve the effect of good antifouling effect.

CN107163254AActive Publication Date: 2017-09-15SHAANXI UNIV OF SCI & TECH
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
Publication Date
2017-09-15

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Abstract

The invention discloses a preparation method of solvent-type hydrophobic and oleophobic fluoroalkyl silicone resin. The preparation method of the hydrophobic and oleophobic fluoroalkyl silicone resin comprises the following steps: carrying out a hydrosilation addition reaction on hydrogen-containing silicone resin, a fluoroalkyl alkene compound, an alkenyl epoxy compounds and alkenyl silane to synthesize a fluoroalkyl / alkyloxy co-modified silicone resin intermediate FR, and carrying out hydrolysis copolycondensation on the intermediate FR, fluoroalkyl halogenosilane and a multifunctional coupling agent with the functionality being not less than 4 in the solvent in the presence of a non-exogenous catalyst in order to prepare the nanometer rough structure embedded hydrophobic and oleophobic fluoroalkyl silicone resin. The fluoroalkyl silicone resin cooperates with an organic tin catalyst, the obtained mixture is diluted with the solvent, the surface of glass or metal or an another substrate is coated with the diluted mixture, and the coated diluted mixture is cured at a high temperature to form a film, so the substrate is endowed with waterproofing and antifouling effects.
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Description

technical field

[0001] The invention belongs to the technical field of silicone resin modification, and in particular relates to a preparation method and application of a solvent-type hydrophobic and oleophobic fluorocarbon-based silicone resin. Background technique

[0002] Fluorosilicone resin, the molecular structure is connected with low surface energy hydrophobic and oleophobic fluorocarbon groups, and oligomeric silsesquioxane [-(SiO 3 / 2 ) x -] The unique dendritic or net-like structure can combine the multiple performance characteristics and advantages of organic fluorine and silicon materials, and can be used in the treatment of glass and metal. It can not only significantly improve the water and oil repellency of the surface of the substrate, but also can It imparts ideal hardness and light transmittance to the treated substrate, so it is widely used in the field of functional transparent coatings or antifouling coatings.

[0003] Hydrosilylation reaction of hydro...

Examples

Embodiment 1

[0028] In a 100mL three-necked flask equipped with a reflux condenser, a thermometer, and a stirrer, add 10g (containing Si-H bond 0.09mol) in sequence (1a), (2a), (1b), (3b), R 1 =R 2 =-CH 3, Si-H content of 0.9mmol / g, methyl hydrogen-containing silicone resin (HSR-1) with a viscosity of 143mPa.s, 32.1g (0.072mol) heptadecafluoro-1-decene (R f17 V), 0.051g (0.00045mol) allyl glycidyl ether (AGE), 4.28g (0.0225mol) vinyltriethoxysilane (VTES), Si-H:R in HSR-1 f17 V:AGE:VTES molar ratio is 1:0.8:0.005:0.25, stir and mix to obtain mixture A; then, mix A with 23.2g (accounting for 50% of the mass of A) co-solvent trifluoroethanol and heat to 80 °C, then add 500ppm complex platinum catalyst KP22 and carry out the hydrosilylation addition reaction at 80°C for 10 hours; after the reaction is over, recover the co-solvent under normal pressure at 85°C, and then decompress and remove the low boiling point for 10min under the condition of 50mmHg , to obtain a total amount of about 46...

Embodiment 2

[0031] In a 100mL three-necked flask equipped with a reflux condenser, a thermometer, and a stirrer, add 20g (containing Si-H bond 0.02mol) in sequence (2a), (2b), (3b), R=-C 12 h 25 , R 1 =R 2 =-CH 3 , Si-H content of 0.1mmol / g, viscosity of 2000mPa.s dodecyl methyl hydrogen-containing silicone resin, 2.77g (0.008mol) tridecafluoro-1-octene (R f13 V), 0.51g (0.004mol) glycidyl acrylate (GA), 0.74g (0.005mol) vinyltrimethoxysilane (VTMS), Si-H in HSR-2: R f13 V: GA: VTMS molar ratio is 1: 0.4: 0.2: 0.25, stir and mix to obtain mixture A; then, A is heated to 80°C, then 250ppm complex platinum catalyst KP23 is added and the temperature is controlled at 100°C for silicon The hydrogenation addition reaction was 2 hours; the reaction was completed, and the low boiling was removed under reduced pressure at 100°C and 260mmHg for 5 minutes to obtain a total amount of about 24.02g tridecafluorooctyl / trimethoxysilyl ethyl co-modified silicone resin (FR- 2) Intermediates.

[0032]...

Embodiment 3

[0034] In a 100mL three-necked flask equipped with a reflux condenser, thermometer, and stirrer, add 12.0g (containing Si-H bond 0.036mol) in sequence (1a), (2a), (2b), (3b), R=-CH 3 , R 1 =R 2 =-ph, Si-H content of 0.3%, viscosity of 1200mPa.s methyl phenyl hydrogen-containing silicone resin (HSR-3, Jiangxi Lvtai Technology Co., Ltd.), 10.08g (0.0252mol) dodecyl methacrylate Fluoroheptyl ester (DFMA), 0.76g (0.0053mol) glycidyl methacrylate (GMA), 0.44g (0.0018mol) 3-(methacryloyloxy)propyltrimethoxysilane (KH-570), Si-H: DFMA: GMA: KH-570 molar ratio in HSR-3 is 1: 0.7: 0.15: 0.05, stir and mix well to obtain mixture A; then, heat A to 80°C, and then add 100ppm platinum catalyst KP22 And the temperature was controlled at 90°C to carry out the hydrosilylation addition reaction for 4 hours; after the reaction was completed, under the condition of 210mmHg, the low boiling was removed for 7 minutes, and the total amount was about 23.28g of dodecafluoroheptoxyacylpropyl / trimet...