A kind of synthetic method of ultraviolet absorber uva Plus
A synthesis method and technology for an absorbent, which are applied in the field of preparation of ultraviolet absorbents, can solve the problems of high production cost, excessively dark product color, difficulty in refining, etc., and achieve the effects of low production cost, low industrial cost, and simple refining and purification.
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Embodiment 1
[0034] A kind of synthetic method of ultraviolet absorber UVA Plus, comprises the steps:
[0035] (1) Esterification reaction: Add 29.6 g of phthalic anhydride and 35.5 g of n-hexanol into a three-necked flask, stir and dissolve at room temperature, and react at 25°C for 2 hours. After cooling to room temperature, 50.0 g of monohexyl phthalate was obtained, with a synthetic yield of 100%, which was directly used in the next acylation reaction without purification;
[0036] (2) Acylation reaction: put 16.5 g of 3-hydroxy-N, N-diethylaniline, 40.0 g of monohexyl phthalate, 15.0 g of anhydrous zinc chloride, and 20.0 g of phosphorus oxychloride into a three-necked flask g and N, N-dimethylformamide 120g, start stirring, stir and dissolve at room temperature, heat up to 70°C, keep warm for 4 hours, hydrogen chloride produced during the reaction is absorbed by the absorption tower, after the reaction is completed, the solvent is recovered under reduced pressure, and then Cool to r...
Embodiment 2
[0042] A kind of synthetic method of ultraviolet absorber UVA Plus, comprises the steps:
[0043] (1) Esterification: Add 340 g of phthalic anhydride and 340 g of n-hexanol into the reactor, stir and dissolve at room temperature, and react for 1 hour at 50° C. At room temperature, 574 g of monohexyl phthalate was obtained, the synthesis yield was 100%, and it was directly used in the next acylation reaction without refining;
[0044] (2) Acylation reaction: 130g of 3-hydroxy-N,N-diethylaniline, 520g of monohexyl phthalate, 130g of anhydrous zinc chloride, 130g of phosphorus oxychloride and dimethyl 1170g of sulfoxide, start stirring, stir and dissolve at room temperature, heat up to 50°C, and keep warm for 5h. The hydrogen chloride produced in the reaction process is absorbed by the absorption tower. Slowly add 1800mL of water, stir until the residue dissolves while adding water, then extract and separate with 570mL ethyl acetate, extract three times, combine the organic phas...
Embodiment 3
[0047] A kind of synthetic method of ultraviolet absorber UVA Plus, comprises the steps:
[0048] (1) Esterification reaction: Add 3.0 kg of phthalic anhydride and 4.2 kg of n-hexanol into the reactor, stir and dissolve at room temperature, and react at 35°C for 3 hours. After cooling to room temperature, 5.1 g of monohexyl phthalate was obtained, the synthesis yield was 100%, and it was directly used in the next acylation reaction without purification;
[0049] (2) Acylation reaction: put 1.5kg of 3-hydroxy-N,N-diethylaniline, 4.0kg of monohexyl phthalate, 1.6kg of anhydrous zinc chloride, and 2.6 kg of phosphorus oxychloride into the reactor kg and N,N-dimethylformamide 12kg, start stirring, stir and dissolve at room temperature, raise the temperature to 80°C, and keep the temperature for 3 hours. The hydrogen chloride produced during the reaction is absorbed by the absorption tower. Cool to room temperature; then slowly add 30L of water into the reaction bottle, stir while...
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