Preparation method of organic fluorosiloxane modified polyurethane emulsion containing short fluoroalkyl chain
A silicon-modified polyurethane and organic fluorine technology, applied in polyurea/polyurethane coatings, coatings, etc., can solve the problems of water resistance, solvent resistance, and solvent environmental pollution, and achieve enhanced water resistance and good water repellency , good heat resistance effect
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Embodiment 1
[0048] Add 3.76g (10mmol) of perfluorohexyl propylene oxide into a completely sealed 100ml single-mouth bottle, 15.53g (0.15mol) of an excess concentration of 30% methylamine aqueous solution, add 50ml of solvent methanol, and stir the mixture for 10h under magnetic force. Remove excess methylamine and solvent methanol by rotary evaporation, then add 4.51 g (12 mmol) of perfluorohexyl propylene oxide and a small amount of methanol, and react under reflux at 65°C for 10 h. The solvent was removed by rotary evaporation, and then recrystallized with chloroform. After cooling, 6.28 g of the target product fluorine-containing dihydric alcohol was obtained, with a yield of 80.26%.
Embodiment 2
[0050] Add 6.65g (30mmol) of isophorone diisocyanate, 20.1g (10.05mmol) of polytetrahydrofuran ether glycol, and 4.2 g (2.1mmol), react at 90°C for 2.5h. Dissolve 1.8g (13.4mmol) of dimethylolpropionic acid and 1.05g (1.35mmol) of fluorine-containing diol in 2.0ml of N-methyl-2-pyrrolidone, add them into the reaction bottle, and react at 90°C for 4h. When the reaction temperature dropped to 40°C, triethylamine (1.35 g, 13.4 mmol) was added to neutralize the reaction, and the reaction was maintained for 30 min. Then the temperature in the reaction bottle was lowered to 0°C, and 80.0g (4.45mol) of water was added to disperse for 1h under the action of a high-speed disperser at a speed of 8000r / min, and 0.3g (4.9mmol) of ethylenediamine was added to extend the chain. An organofluorosilicon-modified aqueous polyurethane solution with a solid content of about 30% was obtained.
Embodiment 3
[0052] Add 6.65g (30mmol) of isophorone diisocyanate, 19.3g (9.65mmol) of polytetrahydrofuran ether glycol, and 3.5g of hydroxyl silicone oil into a 250ml four-necked bottle equipped with a nitrogen drying tube, a reflux condenser, a mechanical stirring paddle, and a thermometer. g (1.75mmol), react at 90°C for 1.5h. Dissolve 1.7g (12.7mmol) of dimethylolpropionic acid and 1.75g (2.2mmol) of fluorine-containing diols in 5.0ml of N-methyl-2-pyrrolidone, add them to the reaction bottle, and react at 90°C for 6h . When the reaction temperature dropped to 40°C, 1.3 g (12.8 mmol) of triethylamine was added to neutralize the reaction, and the reaction was maintained for 30 min. Then the temperature in the reaction bottle was lowered to 0°C, and 95.5g (5.3mol) of water was added to disperse for 1h under the action of a high-speed disperser at a speed of 8000r / min, and 0.3g (4.9mmol) of ethylenediamine was added to extend the chain. An organofluorosilicon-modified aqueous polyuret...
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