Environment-friendly preparation method of 2-chloro-4-nitro-6-bromoaniline
A nitro, aniline technology, applied in the field of dye intermediate preparation, can solve the problems of poor production safety, poor quality, low purity, etc., and achieve the effects of improving material utilization, reducing aminolysis pressure and temperature, and reducing waste acid
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Embodiment 1
[0057] (a) Reaction nitration: Take 291g of nitration waste acid recovered by nitration reaction, add 69g of 105 acid and 81g of nitric acid in turn, and prepare a mixed acid solution of nitric acid: sulfuric acid: water = 1:2:2.2, drop in 180g o-dichlorobenzene Add, o-dichlorobenzene and nitric acid molar ratio is 1:1.21, dropwise temperature is controlled at less than 30 ° C, 60 ° C heat preservation reaction to the end, layered to obtain 233.1 g of nitrated crude product.
[0058] (b) Purification: Add the crude nitrate obtained in step (a) to 585 g of purified and recovered 80% ethanol, heat and stir at 35°C for 1 hour, cool down to 2°C, precipitate and filter to obtain high-purity 3,4-dichloronitronitro Benzene 212.3g, purity 98.9%, ethanol was recovered from the filtrate, the recovered amount was 513g, and the ethanol concentration was 81%.
[0059] (c) Ammonolysis reaction: Add 150 g of high-purity 3,4-dichloronitrobenzene prepared in step (b) into 200 g of water, add 1...
Embodiment 2
[0062] (a) Nitrification reaction: Take 315g of nitrification waste acid recovered by nitrification reaction, add 65 acid 51g, nitric acid 81g successively, be mixed with nitric acid: sulfuric acid: water = 1:2:2.2 mixed acid solution, drop in 180g o-dichlorobenzene Adding, the dropping temperature is controlled at less than 30°C, and the reaction is kept at 60°C until the end point, and 232.9g of the nitrated crude product are obtained by layering.
[0063] (b) Purification: Add the crude nitrate obtained in step (a) to 585 g of purified and recovered 80% ethanol, heat and stir at 35°C for 1 hour, cool down to 2°C, precipitate and filter to obtain high-purity 3,4-dichloronitronitro Benzene 212.3g, purity 99%, ethanol is recovered from the filtrate, the recovered amount is 523g, and the ethanol concentration is 79%.
[0064] (c) Ammonolysis reaction: Add 150 g of high-purity 3,4-dichloronitrobenzene prepared in step (b) into 200 g of water, add 1.5 g of cuprous chloride, 3.5 g...
Embodiment 3
[0067] (a) Nitrification reaction: Take 328g of nitrification waste acid recovered by nitrification reaction, add sulfur trioxide 42.7g, nitric acid 81g successively, be mixed with nitric acid: sulfuric acid: water=1:2:2.2 mixed acid solution, add to 180g o-dichlorobenzene During the dropwise addition, the dropping temperature was controlled at less than 30°C, kept at 60°C until the end point, and 233.1 g of the crude nitration product was obtained by layering.
[0068] (b) Purification: Add the crude nitrated compound obtained in step (a) to 535 g of purified and recovered 82% ethanol, heat and stir at 35°C for 1 hour, cool down to 2°C, precipitate and filter to obtain high-purity 3,4-dichloronitronitro Benzene 213.1g, purity 98,. 5%, ethanol was recovered from the filtrate, the recovery amount was 487g, and the ethanol concentration was 80%.
[0069] (c) Ammonolysis reaction: Add 150 g of high-purity 3,4-dichloronitrobenzene prepared in step (b) into 200 g of water, add 1.5...
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