• 专利标题:   Preparation of p-nitrophenol comprising adding p-nitrochlorobenzene and aqueous sodium hydroxide solution, stirring, raising temperature, adding sulfuric acid solution to obtain reaction solution, separating oil layer by oil-water separation and subjecting oil layer to ultrafiltration.
  • 专利号:   CN114591175-A
  • 发明人:   CAO M, YAO X, XIONG G, HUANG Z, GUO X, CHEN Y, CHEN B
  • 专利权人:   ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO
  • 国际专利分类:   B01D061/14, B01D067/00, B01D071/34, C07C201/12, C07C201/16, C07C205/22
  • 专利详细信息:   CN114591175-A 07 Jun 2022 C07C-201/12 202273 Chinese
  • 申请详细信息:   CN114591175-A CN10152855 18 Feb 2022
  • 优先权号:   CN10152855

▎ 摘  要

NOVELTY - Preparation of p-nitrophenol comprising (i) adding p-nitrochlorobenzene to a reaction kettle, adding15% aqueous sodium hydroxide solution to the reaction kettle, raising the temperature to 157℃, constantly stirring for 1 hour and raising the temperature to 167℃, constantly stirring for 3 hours to obtain primary product and (ii) adding the primary product to the reaction kettle, raising the temperature to 80℃, slowly adding 31% sulfuric acid solution, stirring and reacting the mixture for 30 minutes, reducing the temperature to 45℃ and continuously reacting for 30 minutes to obtain a reaction solution, separating oil layer and water, washing the oil layer with hot water at 60-80℃, separating oil layer and subjecting oil layer to ultrafiltration through an ultrafiltration membrane, where the clear liquid crystallizes to obtain p-nitrophenol. USE - The preparation method is used to produce p-nitrophenol. ADVANTAGE - The production process removes fine impurities, saves resources, greatly improves the quality of produced p-nitrophenol, and increases the yield. DETAILED DESCRIPTION - Preparation of p-nitrophenol comprising (i) adding p-nitrochlorobenzene to a reaction kettle, adding15% aqueous sodium hydroxide solution to the reaction kettle, raising the temperature to 157℃ constantly stirring for 1 hour and raising the temperature to 167℃, constantly stirring for 3 hours to obtain primary product and (ii) adding the primary product to the reaction kettle, raising the temperature to 80℃, slowly adding 31% sulfuric acid solution, stirring and reacting the mixture for 30 minutes, reducing the temperature to 45℃ and continuously reacting for 30 minutes to obtain a reaction solution, separating oil layer and water, washing the oil layer with hot water at 60-80℃, separating oil layer and subjecting oil layer to ultrafiltration through an ultrafiltration membrane, where the clear liquid crystallizes to obtain p-nitrophenol. The ultrafiltration membrane is obtained by soaking polyvinylidene fluoride ultrafiltration membrane in isopropanol for 2 hours, fixing in a splint reaction tank, pouring dopamine solution into the splint reaction tank, and adding 2 mg/mL modified graphene oxide suspension, soaking for 30 minutes, and soaking in deionized water and absolute ethanol for 20 minutes respectively to prepare the ultrafiltration membrane.