Preparation method of p-nitrophenol
A technology of p-nitrophenol and p-nitroaniline, which is applied in the field of preparation of p-nitrophenol, can solve problems such as pressurization, wastewater discharge, high temperature, etc., and achieve the effects of simple treatment method, safe process route, and simple operation steps
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Embodiment 1
[0021] (1) Salt-forming reaction: add 40g of water to a 250ml four-neck flask equipped with a thermometer, a spherical condenser, and mechanical stirring, and slowly add 40g of concentrated sulfuric acid under the condition of rapid stirring and air bath cooling, observe the temperature, and change the temperature of the oil bath. At 120°C, add 13.8g of p-nitroaniline three times, heat up to reflux after addition, react for 10 minutes until the solution is clear, remove the oil bath, air cool to below 50°C, change the water bath to cool to room temperature, a large amount of white solids precipitate out.
[0022] (2) Diazotization reaction: Transfer the reaction solution from the previous step to a low-temperature constant temperature bath, control the temperature to 0-5°C, slowly add a saturated aqueous solution containing 7g of sodium nitrite dropwise, and keep warm for 2 hours after the dropwise addition is completed. Add an appropriate amount of urea to the reaction solutio...
Embodiment 2
[0029] (1) Salt-forming reaction: add 40g of water to a 250ml four-neck flask equipped with a thermometer, a spherical condenser, and mechanical stirring, and slowly add 40g of concentrated sulfuric acid under the condition of rapid stirring and air bath cooling, observe the temperature, and change the temperature of the oil bath. At 120°C, add 13.8g of p-nitroaniline three times, heat up to reflux after addition, react for 10 minutes until the solution is clear, remove the oil bath, air cool to below 50°C, change the water bath to cool to room temperature, a large amount of white solids precipitate out.
[0030] (2) Diazotization reaction: transfer the reaction solution from the previous step to a low-temperature constant temperature bath, and control the temperature to 0-5°C. Slowly add a saturated aqueous solution containing 7g of sodium nitrite dropwise, and keep warm for 2 hours after the dropwise addition. After the warming is over, add an appropriate amount of urea to th...
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