A kind of fluorine-containing polyurethane and preparation method thereof
A technology of polyurethane and fluorine-containing alkyl polyether, applied in the field of polyurethane, can solve problems such as insufficient weather resistance and water resistance, reduce the mechanical properties of polyurethane products, and fail to reach modified polyurethane, etc. Cured, easy to store effect
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Embodiment 1
[0038] (1) Synthesis of nonafluorooxetane monomer
[0039] In a 1000mL three-necked flask equipped with a thermometer, ice-water bath and magnetic stirrer protection, add 16.1g of butyl acetate, 26.2g of sodium bicarbonate, 55.8g of sodium dithionite, 227g of N,N-dimethylformamide, 202g of water, 55.3g of perfluorobutyl iodide was added dropwise, reacted at -13°C for 3h, slowly raised to room temperature, and kept for 2h. After the reaction was completed, extraction was performed three times with 180 g of toluene. The extracts were combined, washed 3 times with water to obtain a solution of 4-nonafluorobutyl-3-iodobutyl acetate, which was added to a 1000mL three-necked flask, and 310g of sodium hydroxide solution with a mass concentration of 20% was added dropwise and kept at React at 12°C for 3h. After the reaction, the layers were separated. The organic layer was washed three times with water, dried and distilled under reduced pressure to obtain 32.6 g of 3-(1H,1H-nonaflu...
Embodiment 2
[0047] (1) Synthesis of nonafluorooxetane monomer
[0048] In a 1000mL three-necked flask equipped with a thermometer, ice-water bath and magnetic stirrer protection, add 16.5g of butyl acetate, 26.4g of sodium bicarbonate, 53.6g of sodium dithionite, 230g of N,N-dimethylformamide, 210g of water was added dropwise with 55.5g of perfluorobutyl iodide, reacted at -15°C for 3h, slowly raised to room temperature, and kept for 2h. After the reaction was completed, extraction was performed three times with 180 g of toluene. The extracts were combined, washed 3 times with water to obtain a solution of 4-nonafluorobutyl-3-iodobutyl acetate, which was added to a 1000mL three-necked flask, and 310g of sodium hydroxide solution with a mass concentration of 20% was added dropwise and kept at React at 11°C for 3h. After the reaction, the layers were separated. The organic layer was washed three times with water, dried and distilled under reduced pressure to obtain 34.2 g of 3-(1H,1H-non...
Embodiment 3
[0056] (1) Synthesis of tridecafluorooxetane monomer
[0057] In a 1000mL three-necked flask equipped with a thermometer, ice-water bath and magnetic stirrer protection, add 16.5g of butyl acetate, 28.2g of sodium bicarbonate, 55.5g of sodium dithionite, 221g of N,N-dimethylformamide, 230g of water, 73.0g of perfluorohexyl iodide was added dropwise, and the addition was completed in 50 minutes. After the addition, it was reacted at -12°C for 6 hours, slowly raised to room temperature, and kept for 3 hours. After the reaction was finished, extract with 180g trifluorotoluene in 3 times. The extracts were combined and washed 3 times to obtain a 4-tridecafluorohexyl-3-iodobutyl acetate solution. The solution was directly added to a 1000mL three-necked flask, and 550g of mass concentration was added dropwise to a 10% sodium hydroxide solution. Insulate and react at 13°C for 8h. After the reaction, the layers were separated. The organic layer was washed three times with water, dr...
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