Benzotriazole-based (co)polymer, ultraviolet-absorbing paint containing same, and film coated with same
A technology of benzotriazole series and polymers, applied in the direction of radiation-absorbing coatings, coatings, chemical instruments and methods, etc., can solve the problems of insufficient ultraviolet shielding function, low absorption, difficult to use, etc., and achieve ultraviolet absorption performance Excellent effect with less coloring and excellent absorption performance
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[0063] Hereinafter, the present invention will be described in more detail with examples and comparative examples of benzotriazole-based (co)polymers, coating materials and coating-coated films including these examples, but the present invention is not limited to these embodiments. In addition, "%" described in a synthesis example, an Example, and a comparative example shows "weight%", and "part" shows a "weight part."
[0064] [1. Synthesis of benzotriazole-based monomers]
Synthetic example 1
[0066] [Intermediate (a): Synthesis of 5-carboxy-2-(2-hydroxy-4-methoxyphenyl)-2H-benzotriazole]
[0067] [Chem 3]
[0068]
[0069] Install spherical condenser, thermometer, stirring device on the four-necked flask of 2000ml, add water 875ml, sodium carbonate 56.5g (0.533 mole), 178.8g (0.982 mole) of 4-amino-3-nitrobenzoic acid and make it dissolve, 197.1 g (1.028 mol) of 36% sodium nitrite aqueous solution was added. Install a spherical condenser, a thermometer, and a stirring device on a 3000ml four-necked flask, add 875ml of water, 372.0g (2.370 moles) of 62.5% sulfuric acid and mix them, cool to 3-7°C to obtain the product, and add the above-mentioned The product was stirred at the same temperature for 1 hour to obtain an aqueous diazonium salt solution. Install a spherical condenser, a thermometer, and a stirring device on a 5000ml four-necked flask, add 139.4g (1.009mol) of 1,3-dimethoxybenzene, 900ml of isopropanol, and 390ml of water and mix them, drop them at 5...
Synthetic example 2
[0073] [Intermediate (b): Synthesis of 5-carboxy-2-(2-hydroxy-4-methoxyphenyl)-2H-benzotriazole]
[0074] [chemical 4]
[0075]
[0076] Install a spherical condenser, a thermometer, and a stirring device on a 2000ml four-necked flask, add 107.1g (0.358 moles) of 5-carboxy-2-(2,4-dimethoxyphenyl)-2H-benzotriazole, 540ml of acetic acid, 365.2g (2.327 moles) of 62.5% sulfuric acid, and 221.8g (2.148 moles) of 95% sulfuric acid were stirred at 130-140°C for 20 hours, then 480ml of water was added, and the precipitate was filtered and washed with water to obtain crude crystals. The resulting crude crystals were reslurried and washed with 130 ml of isopropanol and 300 ml of 4-methyl-2-pentanone to obtain 5-carboxy-2-(2-hydroxyl-4-methoxyphenyl)-2H - Benzotriazole 59.5 g. The yield was 58% (calculated based on 5-carboxy-2-(2,4-dimethoxyphenyl)-2H-benzotriazole).
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