• 专利标题:   Schiff base palladium catalyst includes graphene oxide, Schiff base ligand, catalyst carrier, and main active components palladium salt, where active component includes palladium.
  • 专利号:   CN103447092-A, CN103447092-B
  • 发明人:   HUANG B, YUAN D, CHEN B, QIAN Y, LIAO S, ZHANG Q, CAI Q, YANG M, YUAN L
  • 专利权人:   UNIV EAST CHINA TECHNOLOGY
  • 国际专利分类:   B01J031/22, C07B037/00, C07C051/353, C07C057/44
  • 专利详细信息:   CN103447092-A 18 Dec 2013 B01J-031/22 201420 Pages: 11 Chinese
  • 申请详细信息:   CN103447092-A CN10416149 13 Sep 2013
  • 优先权号:   CN10416149

▎ 摘  要

NOVELTY - Schiff base palladium catalyst includes a graphene oxide, Schiff base ligand, catalyst carrier, and a main active components palladium salt, where the active component includes 5.0-10.0 % of palladium. The graphene oxide has a particle diameter of 1-5 microns and thickness of 0.8-1.2 nm, where the palladium nanoparticle has a diameter of 3-8 nm. The catalyst carrier is prepared by cooling 200-300 parts of concentrated sulfuric acid at 0 to -0.5 degrees C in an ice bath. USE - Schiff base palladium catalyst. ADVANTAGE - The Schiff base palladium catalyst prevents loss of palladium in catalytic process, improves palladium nanoparticles dispersion, enhances load-type catalytic activity, and good repeating use performance in C-C coupling reaction process. DETAILED DESCRIPTION - Schiff base palladium catalyst includes a graphene oxide, Schiff base ligand, catalyst carrier, and a main active components palladium salt, where the active component includes 5.0-10.0 % of palladium. The graphene oxide has a particle diameter of 1-5 microns and thickness of 0.8-1.2 nm, where the palladium nanoparticle has a diameter of 3-8 nm. The catalyst carrier is prepared by cooling 200-300 parts of concentrated sulfuric acid at 0 to -0.5 degrees C in an ice bath, in which 5-15 parts of graphite powder and 5-15 parts of sodium nitrate are added slowly in the cooled sulfuric acid to form a mixture. 30-50 parts of potassium permanganate is also added for maintaining temperature of the reaction system at 20 degrees C, where the reaction mixture is uniformly stirred for 120-180 minutes and then 500-1000 parts of deionized water is also added to set temperature of the reaction system not more than 98 degrees C. The reaction system is continuously stirred for 15-30 minutes, in which 600-800 parts of deionized water and 50-100 parts of 30% hydrogen peroxide are also added. The formed reaction mixture is filtered to form filter cake, which is washed with deionized water and centrifuged to obtain catalyst carrier sample. The obtained catalyst carrier sample is frozen and dried to obtain black graphene oxide powder. An INDEPENDENT CLAIM is included for a method for preparing Schiff base palladium catalyst, which involves: (A) mixing 200-300 parts of concentrated sulfuric acid, 5-15 parts of graphite powder, 5-15 parts of sodium nitrate, and 30-50 parts of potassium permanganate during stirring slowly; (B) maintaining temperature of reaction system not more than 20 degrees C for 120-180 minutes; (C) adding 500-1000 parts of deionized water and 50-100 parts of 30% hydrogen peroxide at 98 degrees C for 15-30 minutes to form black graphene oxide powder; (D) adding 0.1-0.5 parts of graphene oxide into 100-400 parts of aliphatic amine or aromatic amine in N,N dimethylformamide; (E) performing ultrasonic oscillation for 120-240 minutes; (F) adding 1-5 parts of dicyclohexyl carbodiimide and 1-5 parts of N-hydroxy succinic imide during stirring at 60-80 degrees C for 360-720 minutes; (G) cooling the reaction mixture at room temperature to form a product; (H) isolating the formed product by centrifugation; (I) washing the isolated product successively with ethanol and distilled water; (J) freezing and drying the washed product to obtain black powder of amidated graphene oxide; (K) preparing Schiff base loaded graphite oxide by adding 0.1-0.5 parts of the formed amidated graphene oxide to an ethanol solution containing 100-400 parts of an aldehyde compound or a ketone compound; (L) performing ultrasonic vibration for 60-120 minutes; (M) refluxing the reaction mixture for 360-720 minutes at room temperature to form a product; (N) isolating the formed product by centrifugation; (O) washing the isolated product successively with ethanol and distilled water; (P) freezing and drying the washed product to obtain a black powder loaded with graphene oxide; (Q) mixing 0.1-0.5 parts of the formed graphene oxide the with 50-100 parts of ethanol solution of palladium salt at room temperature; and (R) filtering the reaction mixture by using magnetic separation after freeze-drying to form the Schiff base palladium catalyst.