• 专利标题:   Preparing graphene-loaded palladium nano-particle composite catalyst by soaking graphene oxide aqueous solution in palladium chloride solution, reacting, dissolving palladium acetate with absolute ethanol, adding bromobenzene and reacting.
  • 专利号:   CN111589443-A
  • 发明人:   HE J, JIANG Y, YAO C, PANG F, LI J, YI W
  • 专利权人:   SINO PLATINUM METALS CO LTD
  • 国际专利分类:   B01J023/44, B01J037/02, B01J037/18, B01J038/48, B01J038/52, C07C001/32, C07C015/14
  • 专利详细信息:   CN111589443-A 28 Aug 2020 B01J-023/44 202076 Pages: 8 Chinese
  • 申请详细信息:   CN111589443-A CN10462942 27 May 2020
  • 优先权号:   CN10462942

▎ 摘  要

NOVELTY - Method for preparing graphene-loaded palladium nano-particle composite catalyst, involves (i) taking graphene oxide aqueous solution, putting into palladium chloride solution, and soaking, (ii) drying the obtained mixed solution using spray-drying equipment and collecting graphene oxide powder containing palladium, (iii) subjecting the palladium-containing graphene oxide powder to high temperature reduction in a hydrogen atmosphere in a tube furnace, (iv) weighing palladium acetate, dissolving with 1:1 absolute ethanol and deionized water, weighing palladium-containing graphene powder and putting into the above solution, maintaining at 30-50 degrees C, and continuously stirring for 3-6 hours, (v) putting phenylboronic acid, bromobenzene, and cesium carbonate into a palladium-containing solution, raising the temperature to 80 degrees C, stirring to react for 1-4 hours, tracking the reaction situation by thin-layer chromatography, and cooling to room temperature. USE - The method is useful for preparing graphene-loaded palladium nano-particle composite catalyst. ADVANTAGE - The method is simple and has mild condition. The catalyst has high activity and can be reused many times. DETAILED DESCRIPTION - Method for preparing graphene-loaded palladium nano-particle composite catalyst, involves (i) taking carrier and palladium based on a mass ratio of (400-1000):1, taking graphene oxide aqueous solution, putting into a certain concentration of palladium chloride solution, and soaking for 24-48 hours, (ii) drying the obtained mixed solution using spray-drying equipment under atomization liquid flow rate of 3-8 ml/minute, atomization pressure of 0.1-0.5 MPa, inlet temperature of 170-190 degrees C, and hot air flow rate of 4-10 l/minute, and collecting graphene oxide powder containing palladium, (iii) subjecting the palladium-containing graphene oxide powder to high temperature reduction in a hydrogen atmosphere in a tube furnace, (iv) weighing palladium acetate, dissolving with 1:1 absolute ethanol and deionized water, weighing palladium-containing graphene powder and putting into the above solution, maintaining at 30-50 degrees C, and continuously stirring for 3-6 hours, (v) putting phenylboronic acid, bromobenzene, and cesium carbonate into a palladium-containing solution, where the molar ratios of palladium acetate, phenylboronic acid, bromobenzene, and cesium carbonate is 0.05:1:1.25:3 respectively, raising the temperature to 80 degrees C, stirring to react for 1-4 hours, tracking the reaction situation by thin-layer chromatography, and cooling to room temperature, where the catalyst comprises graphene carrier and palladium nanoparticles supported on the carrier, and the content of palladium is 1-2.5 wt.%.