• 专利标题:   Preparation of graphene loaded high-dispersion nano nickel catalyst for selective catalytic hydrogenation of cinnamic aldehyde, involves mixing graphite with concentrated sulfuric acid, sodium nitrate and potassium permanganate.
  • 专利号:   CN103301841-A, CN103301841-B
  • 发明人:   LI F, MA Q, FAN G
  • 专利权人:   UNIV BEIJING CHEM TECHNOLOGY
  • 国际专利分类:   B01J023/755, C07C045/62, C07C047/228
  • 专利详细信息:   CN103301841-A 18 Sep 2013 B01J-023/755 201403 Chinese
  • 申请详细信息:   CN103301841-A CN10069361 15 Mar 2012
  • 优先权号:   CN10069361

▎ 摘  要

NOVELTY - Preparation of graphene loaded high-dispersion nano nickel catalyst involves mixing graphite with concentrated sulfuric acid, sodium nitrate and potassium permanganate in mass ratio of 1:0.5-1:15-30:2-5 for 0.5-1.5 hours, warming to 20-40 degrees C, then adding graphite and deionized water in mass ratio of 1:40-100, adding deionized water, heated to 90-100 degrees C for 0.5-6 hours, then adding graphite, deionized water and 30% hydrogen peroxide in weight ratio of 1:90-130:5-11, centrifuging, washing with dilute hydrochloric acid and deionized water until neutral. USE - Preparation of graphene loaded high-dispersion nano nickel catalyst used for selective catalytic hydrogenation of cinnamic aldehyde (claimed). ADVANTAGE - The method efficiently and economically provides graphene loaded high-dispersion nano nickel catalyst. The cinnamic aldehyde is obtained using the catalyst with reaction conversion rate of 86-100% and selectivity of 88-96%. DETAILED DESCRIPTION - Preparation of graphene loaded high-dispersion nano nickel catalyst involves mixing graphite with concentrated sulfuric acid, sodium nitrate and potassium permanganate in mass ratio of 1:0.5-1:15-30:2-5 for 0.5-1.5 hours, warming to 20-40 degrees C, then adding graphite and deionized water in mass ratio of 1:40-100, adding deionized water, heated to 90-100 degrees C for 0.5-6 hours, then adding graphite, deionized water and 30% hydrogen peroxide in weight ratio of 1:90-130:5-11, centrifuging, washing with dilute hydrochloric acid and deionized water until neutral, drying at 60-80 degrees C and obtaining graphite oxide, dispersing obtained 1-5 mg/mL graphite oxide in deionized water, ultrasonically-treating for 1-4 hours, allowing to standstill for 12-24 hours, centrifuging supernatant at 3000-4000 rpm for 5-15 minutes, and obtaining graphene oxide solution, then adding aqueous nickel nitrate solution and aluminum nitrate mixed salt solution having nickel nitrate content of 0.1-0.3 mol/L, aluminum nitrate content of 0.05-0.3 mol/L, where nickel nitrate and aluminum nitrate molar ratio is 1-3:1, mixing, ultrasonically-dispersing for 30-60 minutes, adding alkaline solution, adjusting pH to 10-12, crystallizing at 80-100 degrees C for 12-24 hours, cooling to room temperature, filtering, washing filter cake with deionized water until neutral, drying in oven at 40-60 degrees C for 12-24 hours and obtaining graphene/nickel-aluminum layered double hydroxide complex, and processing obtained compound in a tubular atmosphere furnace under nitrogen atmosphere at 500-700 degrees C for 1-4 hours with rate of 5-10 degrees C/minute.