Photochromic water-repellent non-woven fabric and preparation method thereof
A photochromic material and photochromic technology, applied in the direction of color-changing fluorescent materials, chemical instruments and methods, textiles and papermaking, etc., to achieve the effects of simple process, high production efficiency and simple process
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[0024] The preparation method of the above-mentioned photochromic water-repellent textile fabric of the present invention comprises the following steps:
[0025] 1) Dissolve 1-nitroso-2,7-dihydroxynaphthalene in ethanol, pass nitrogen gas and heat to 80~100℃ under reflux, add 1,3,3-trihydroxynaphthalene dropwise after 5~30 minutes The mixed solution of methyl-2-methylene indoline and ethanol was added dropwise within 15~60 minutes, kept in a reflux state in a nitrogen atmosphere and kept stirring, the reaction was completed after 1~10h, and 5~10% activated carbon was added Reflux for 5 to 30 minutes, filter while hot, distill the filtrate under reduced pressure, remove most of the ethanol, let it cool naturally and stand overnight, filter the precipitated product and wash or recrystallize it with ethanol for many times, and finally obtain off-white after drying in a vacuum oven Solid N-methyl-3,3-dimethyl-9'-hydroxyspiro[2H-indole-2,3'-[3H]naphtho[2,1-b][1,4]oxazine] , wherei...
Embodiment 1
[0031]Dissolve 5.67g (0.03mol) 1-nitroso-2,7-dihydroxynaphthalene in 140mL ethanol, pass nitrogen and heat to 90°C under reflux, add 5.2g (0.03mol) 1 dropwise after 15 minutes , The mixed solution of 3,3-trimethyl-2-methylene indoline and 25 mL of ethanol was added dropwise within 30 minutes. Reflux was maintained under nitrogen with constant stirring. After 5 hours, the reaction was completed, 5% activated carbon was added to reflux for 15 minutes, filtered while hot, and the filtrate was distilled under reduced pressure to remove most of the ethanol, and allowed to cool naturally and stand overnight. The precipitated product was filtered and washed with ethanol for several times or recrystallized. After drying in a vacuum oven, an off-white solid N-methyl-3,3-dimethyl-9'-hydroxyspiro[2H-indole-2,3'-[ was finally obtained. 3H]naphtho[2,1-b][1,4]oxazine]. Mix 1.23g PVDF with 0.012g spirooxazine, dissolve in a mixed solution of 3mL acetone and 7mL DMF, dissolve at 40°C for 2h...
Embodiment 2
[0043] Dissolve 5.67g (0.03mol) 1-nitroso-2,7-dihydroxynaphthalene in 140mL ethanol, pass nitrogen and heat to 90°C under reflux, add 5.2g (0.03mol) 1 dropwise after 15 minutes , The mixed solution of 3,3-trimethyl-2-methylene indoline and 25 mL of ethanol was added dropwise within 30 minutes. Reflux was maintained under nitrogen with constant stirring. After 5 hours, the reaction was completed, 5% activated carbon was added to reflux for 15 minutes, filtered while hot, and the filtrate was distilled under reduced pressure to remove most of the ethanol, and allowed to cool naturally and stand overnight. The precipitated product was filtered and washed with ethanol for several times or recrystallized. After drying in a vacuum oven, an off-white solid N-methyl-3,3-dimethyl-9'-hydroxyspiro[2H-indole-2,3'-[ was finally obtained. 3H]naphtho[2,1-b][1,4]oxazine]. 1.23g PVDF was mixed with 0.008g, 0.01g, 0.012g, 0.014g, 0.016g spirooxazine, respectively, and dissolved in a mixed sol...
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