2-amino-4-nitrophenol synthesis method
A technology of nitrophenol and synthesis method, which is applied in the preparation of amino hydroxy compounds, chemical instruments and methods, preparation of organic compounds, etc. The effect of high safety
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Embodiment 1
[0027] first step,
[0028] Mix 109 kilograms of o-aminophenol and 440 kilograms of dichloroethane in a 1500L reactor, stir, and add 118 kilograms of hydrochloric acid with a mass fraction of 31% in the kettle, after adding the hydrochloric acid, continue stirring;
[0029] second step,
[0030] Keep the reaction temperature constant at 10-15°C, add 101 kilograms of 65% nitric acid to the above reaction kettle, after adding the nitric acid, continue stirring until the content of o-aminophenol is lower than 0.2%;
[0031] third step,
[0032] In the mixture obtained in the second step, adding mass fraction is 15% sodium hydroxide solution to about system pH=8, distillation reclaims 480 kilograms of dichloroethane, and then adding mass fraction is 31% hydrochloric acid to the distillation residue. The pH of the system is 4-5. After filtration, 141.7 kg of 2-amino-4-nitrophenol with a purity of 98.7% and about 413 kg of saline waste water are obtained.
[0033] The about 413 k...
Embodiment 2
[0035] first step,
[0036] Mix 109 kilograms of o-aminophenol and 327 kilograms of dichloromethane in a 1000L reactor, stir, add 50 kilograms of sulfuric acid with a mass fraction of 98% in the kettle, after adding the sulfuric acid, continue stirring;
[0037] second step,
[0038] Keep the reaction temperature constant at 10-15°C, add 95 kg of 65% nitric acid into the above reaction kettle, after the addition of nitric acid, continue stirring until the content of o-aminophenol is lower than 0.1%;
[0039] third step,
[0040] In the mixture obtained in the second step, adding mass fraction is 30% sodium hydroxide solution to about system pH=8, distillation reclaims 350 kg of dichloroethane, and then adding mass fraction is 31% hydrochloric acid to The pH of the system is 4-5. After filtration, 140.7 kg of 2-amino-4-nitrophenol with a purity of 99.3% and about 250 kg of saline waste water are obtained.
[0041] About 250 kilograms of saline waste water that the 3rd step o...
Embodiment 3
[0043] first step,
[0044] Mix 600 kilograms of o-aminophenol and 3000 kilograms of chloroform in a 5000L reaction kettle, stir, add 306 kilograms of sulfuric acid with a mass fraction of 98% in the kettle, after adding the sulfuric acid, continue stirring;
[0045] second step,
[0046] Under the condition of 10±2°C, add 550 kilograms of 65% nitric acid to the mixture obtained in the first step, and the addition is completed;
[0047] third step,
[0048] Add liquid caustic soda to the mixture obtained in the second step, adjust the pH of the system to about 8, reclaim 3380 kg of chloroform by distillation, add hydrochloric acid with a mass fraction of 31% to the system pH of 4 to 5 in the distillation residue, filter to obtain 830 Kg of 2-amino-4-nitrophenol with a purity of 99.1% and about 1200 kg of saline waste water.
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