• 专利标题:   Nitrogen-doped graphene-supported nickel-based catalyst used for selective hydrogenation of phenol to cyclohexanone comprises nitrogen-doped graphene as carrier and supporting active metal nickel.
  • 专利号:   CN112371157-A, CN112371157-B
  • 发明人:   XU H, HUANG G, WU P
  • 专利权人:   UNIV XIAN SHIYOU
  • 国际专利分类:   B01J027/24, B01J035/10, C07C045/00, C07C049/403
  • 专利详细信息:   CN112371157-A 19 Feb 2021 B01J-027/24 202128 Pages: 9 Chinese
  • 申请详细信息:   CN112371157-A CN11374334 30 Nov 2020
  • 优先权号:   CN11374334

▎ 摘  要

NOVELTY - A nitrogen-doped graphene-supported nickel-based catalyst comprises nitrogen-doped graphene as carrier and supporting active metal nickel. The catalyst is prepared by adding graphene oxide to deionized water, ultrasonicating to obtain graphene oxide dispersion, adding nitrogen source, ultrasonically stirring, adding to reaction kettle, and hydrothermally reacting; centrifuging, removing solids from bottom layer, suction filtering, washing with deionized water and absolute ethanol repeatedly wash until neutralized, and vacuum oven drying oven to obtain nitrogen-doped graphene; and dropping nickel nitrate aqueous solution, stirring, soaking overnight, stirring, evaporating water, drying, calcining, and subjecting to reduction reaction under hydrogen atmosphere. USE - The nitrogen-doped graphene-supported nickel-based catalyst is used for selective hydrogenation of phenol to cyclohexanone (claimed). ADVANTAGE - The method has low cost. The catalyst has high specific surface area, good synergy between the carrier and active metal, mild reaction conditions, phenol conversion rate of up to 92.62%, cyclohexanone selectivity of up to 61.75%, good catalytic activity, and high selectivity. DETAILED DESCRIPTION - A nitrogen-doped graphene-supported nickel-based catalyst comprises nitrogen-doped graphene as carrier and 10-30 wt.% supporting active metal nickel based on 100% mass of catalyst. The catalyst is prepared by adding graphene oxide to deionized water, ultrasonicating for 1.5-2.5 hours to obtain graphene oxide dispersion, adding nitrogen source at mass ratio of 1:10-1:50, ultrasonically stirring at room temperature for 0.5-1 hour, adding to reaction kettle, and hydrothermally reacting to 150-200 degrees C for 10-14 hours; centrifuging, removing solids from bottom layer, suction filtering, washing with deionized water and absolute ethanol repeatedly wash until neutralized, and vacuum oven drying oven to obtain nitrogen-doped graphene; and dropping nickel nitrate aqueous solution, stirring for 1-3 hours, soaking overnight, stirring, evaporating water at 60-80 degrees C, drying at 60-80 degrees C, calcining to 300-500 degrees C for 3-5 hours under nitrogen atmosphere, and subjecting to reduction reaction at 300-500 degrees C under hydrogen atmosphere. The nitrogen source is urea, ammonium oxalate, ammonia, ammonium carbonate and/or ammonium bicarbonate. An INDEPENDENT CLAIM is included for selective hydrogenation of phenol to cyclohexanone comprising adding phenol aqueous solution and catalyst at mass ratio of 1:0.2-0.5 into reaction kettle, and hydrogenating to 130-170 degrees C at 0.3-0.5 MPa for 1-3 hours.