• 专利标题:   Preparing reduced palladium-graphene oxide catalyst useful in N-methyl-4-aminoanisole reaction for hydrogenation of N-methylene-4-aminoanisole, comprises e.g. adding palladium chloride and distilled water into concentrated hydrochloric acid.
  • 专利号:   CN107433198-A
  • 发明人:   LI X, SHU Z, YANG H, ZHU F, YIN Y, YANG W
  • 专利权人:   UNIV CHONGQING
  • 国际专利分类:   B01J023/44, B01J037/08, B01J037/18, B01J037/34, C07C213/02, C07C217/84
  • 专利详细信息:   CN107433198-A 05 Dec 2017 B01J-023/44 201809 Pages: 9 Chinese
  • 申请详细信息:   CN107433198-A CN10696114 15 Aug 2017
  • 优先权号:   CN10696114

▎ 摘  要

NOVELTY - Preparing reduced palladium-graphene oxide (Pd-RGO) catalyst comprises adding palladium chloride and distilled water in 10 mg/ml concentrated hydrochloric acid solution of palladium chloride, where mass ratio of palladium chloride and reducing graphene oxide is 1:4, adding palladium chloride solution into reduced graphene oxide, performing ultrasonic dispersion to form mixture, adjusting pH of mixture to 9-10 by sodium hydroxide, allowing to stand for adsorption, filtering and drying to obtain a powder, heating at 300 degrees C for 2 hours and carrying out hydrogen reduction at 300 degrees C for 3 hours. USE - The catalyst is useful in N-methyl-4-aminoanisole reaction for hydrogenation of N-methylene-4-aminoanisole (claimed); and useful in petrochemical industry, pharmaceutical industry, electronic industry, perfumery industry and dye industry. ADVANTAGE - The catalyst has uniformly distributed components, strong adhesive force, high purity without impurities and has excellent catalytic performance. The method is simple, has cheap reaction material, and ensures high palladium loading amount. DETAILED DESCRIPTION - INDEPENDENT CLAIMS are also included for: (1) use of catalyst in the N-methyl-4-aminoanisole reaction for hydrogenation of N-methylene-4-aminoanisole; and (2) synthesizing N-methyl-4-amino-anisole, comprising taking p-methoxy aniline and formaldehyde as reactants at room temperature, and taking tetrahydrofuran as solvent under electromagnetic stirring for 1-5 minutes to obtain an intermediate reaction liquid, where the molar ratio of p-methoxyaniline and formaldehyde is 1:0.5-1:3, stirring under electromagnetic conditions at a speed of 80 revolutions/minute (rpm), subjecting the reaction intermediate to rotary evaporation at 40 degrees C until a brown oily liquid or solid brown precipitate appears at the rotational speed of 80-120 rpm, dissolving the obtained brown oily liquid or solid brown precipitate in methylene chloride solvent and passing through a neutral alumina column to obtain yellow needles, dissolving yellow needles in tetrahydrofuran solvent and stirring and adding palladium on carbon catalyst under 0.1-9 Mpa hydrogen atmosphere pressure and carrying out hydrogenation reduction reaction for 1-6 hours.