• 专利标题:   Preparing p-hydroxyacetophenone comprises adding phenol and modified catalyst into acylation kettle, dropping acetyl chloride under vacuum, cooling, hydrolyzing, water washing, separating water layer, distilling, freezing and crystallizing and centrifuging.
  • 专利号:   CN114163317-A
  • 发明人:   HUANG Q, ZENG Q, LIU Z, ZHENG J
  • 专利权人:   JIANGXI YONGTONG TECHNOLOGY CO LTD
  • 国际专利分类:   B01J029/06, B01J035/10, C07C045/45, C07C049/825
  • 专利详细信息:   CN114163317-A 11 Mar 2022 C07C-045/45 202271 Chinese
  • 申请详细信息:   CN114163317-A CN11508947 10 Dec 2021
  • 优先权号:   CN11508947

▎ 摘  要

NOVELTY - Preparing p-hydroxyacetophenone comprises taking phenol and acetyl chloride as raw materials and using modified catalyst as catalyst. The preparation of the modified catalyst comprises (a) mixing the graphene oxide with water, dispersing uniformly, adding n-butylamine, stirring uniformly, adding aluminum isopropoxide and sodium silicate, using ethanol and deionized water to wash, transferring to the high pressure reaction kettle of polytetrafluoroethylene lining, crystallizing, roasting, (b) using ammonium chloride aqueous solution to exchange the material A, calcining, (c) mixing citric acid, oxalic acid and water to obtain acid solution, mixing the material B with the acid solution, (d) mixing the lithium nitrate, ferric nitrate, cerium nitrate and water to obtain metal salt solution, mixing the metal salt solution with the material C, filtering and washing, drying, roasting to obtain the material D and (e) mixing the material D with phosphotungstic acid and ball milling. USE - The method is useful for preparing p-hydroxyacetophenone. ADVANTAGE - The method: uses catalyst to shorten the reaction time; has high catalytic activity, high product selectivity and does not generate more by-product. DETAILED DESCRIPTION - Preparing p-hydroxyacetophenone comprises taking phenol and acetyl chloride as raw materials and using modified catalyst as catalyst. The preparation of the modified catalyst comprises (a) mixing the graphene oxide with water, dispersing uniformly, adding n-butylamine, stirring uniformly, adding aluminum isopropoxide and sodium silicate, stirring for 30-60 miuntes at 25-30℃, raising the temperature to 70-85℃ and stirring for 3-5 hours, using ethanol and deionized water to wash, transferring to the high pressure reaction kettle of polytetrafluoroethylene lining, raising the temperature to 100-130℃, crystallizing for 10-20 hours, raising the temperature to 150-185℃ and crystallizing for 10-30 hours, washing by ethanol and deionized water, drying, roasting for 30-60 minutes at 400-500℃, roasting for 2-5 hours at the temperature of 550-650℃ to obtain the material A, (b) using ammonium chloride aqueous solution to exchange the material A, calcining for 2-5 hours at 500-600℃ to obtain the material B, (c) mixing citric acid, oxalic acid and water to obtain acid solution, mixing the material B with the acid solution, raising the temperature to 70-80℃, stirring for 9-20 hours, water washing to neutral, drying to obtain the material C, (d) mixing the lithium nitrate, ferric nitrate, cerium nitrate and water to obtain metal salt solution, mixing the metal salt solution with the material C, stirring for 5-12 hours at 55-80℃, allowing to stand for 1-3 hours, filtering and washing, drying, roasting for 1-3 hours at 400-450℃, roasting for 3-8 hours at 500-600℃ to obtain the material D and (e) mixing the material D with phosphotungstic acid and ball milling to obtain he modified catalyst.