Response type ultraviolet absorption agent, synthesized midbody and application thereof
A UV absorber, reactive technology, used in textiles and papermaking, fiber processing, organic chemistry, etc., can solve the problems of poor anti-ultraviolet radiation performance, lack of reactive functional groups, and unsatisfactory fabric fastness. Simple and easy application process, good anti-ultraviolet effect, good fastness effect
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Embodiment 1
[0040] preparation.
[0041] synthetic route:
[0042]
[0043] Synthesis of Intermediate 1: Add 20g of p-nitrophenol, 6g of sodium hydroxide and 200ml of water into a 500ml four-neck flask, heat until dissolved, add 150g of dibromoethane, 1g of tetrabutylammonium bromide, and heat at 90°C React for 12 hours. After the reaction is over, remove water and dibromoethane under reduced pressure, dissolve the residue with hot ethanol, remove undissolved salts, cool, and the product is precipitated from ethanol to obtain 28.3 g of product; yield: 82%. The melting point of the product is 64°C, which is the target product;
[0044] Synthesis of intermediate 2: 8g of intermediate 1 and 80ml of NN-dimethyldodecylamine were reacted at 60°C for 41h, and the crude product was washed with cyclohexane to obtain 14.17g of intermediate 2, with a yield of 95%;
[0045] The structure of intermediate 2 was determined:
[0046] MP: 105-106°C;
[0047] IR (KBr, cm -1 ): 2920, 2840 (CH 3 (...
Embodiment 2
[0063]
[0064] The synthesis of intermediates 1, 2 and 3 is shown in Example 1;
[0065] Synthesis of UV absorber 5: 15ml of water was placed in a reactor, 0.371g (2.0mmol) of tripolychlorazine was dissolved in 10ml of acetone, added to the reactor, and stirred. Dissolve 0.277g (2.0mmol) of anthranilic acid in water, add 10% NaCO 3 Adjust the pH to 7-8, add the prepared sodium salt solution dropwise into the reactor, and at the same time adjust the pH to 6.5-7 with 10% sodium carbonate aqueous solution, finish adding in 1 hour, react at 10°C for 2.5 hours, shrink The reaction is over. Dissolve 0.858g of intermediate 3 in water, add the aqueous solution dropwise into the reactor, adjust the pH to 7.5 with 10% aqueous sodium carbonate solution, and raise the temperature to about 50°C at the same time, and react for 4 hours. After the reaction, salt out with sodium chloride, filter out the precipitate, wash with saturated brine, and dry to obtain 1.205 g, with a yield of 86...
Embodiment 3
[0072]
[0073] The synthesis of intermediates 1, 2 and 3 is shown in Example 1;
[0074] Synthesis of UV absorber 6: 15ml of water was placed in a reactor, 0.371g (2.0mmol) of tripolychlorazine was dissolved in 10ml of acetone, added to the reactor, and stirred. Dissolve 0.328 g (2.0 mmol) of p-aminobenzoic acid dimethylamine in acetone, add it dropwise to the reactor, and adjust the pH to 6.5-7 with 10% aqueous sodium carbonate solution at the same time, add it in 1 hour, and react at 10°C After 3 hours of reaction, the shrinkage reaction ends. Dissolve 0.858g of intermediate 3 in water, add the aqueous solution dropwise into the reactor, adjust the pH to 7.5 with 10% aqueous sodium carbonate solution, and raise the temperature to about 50°C at the same time, and react for 5.5h. After the reaction, the solid was filtered out, and the solid was washed with water and cyclohexane to obtain 1.140 g of the product with a yield of 81%.
[0075] Overall yield of UV absorber 6:...
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