• 专利标题:   Preparing graphene oxide-loaded zirconium iron nano-material useful for catalyzing organophenols to carry out nitrosation reaction on aromatic ring, comprises e.g. dissolving tetrabutyl zirconate in ethanol solution.
  • 专利号:   CN108976130-A, CN108976130-B
  • 发明人:   ZHANG L
  • 专利权人:   ZHANG L
  • 国际专利分类:   B01J023/745, B01J037/10, C07C201/08, C07C205/60
  • 专利详细信息:   CN108976130-A 11 Dec 2018 C07C-205/60 201904 Pages: 9 Chinese
  • 申请详细信息:   CN108976130-A CN11096802 20 Sep 2018
  • 优先权号:   CN11096802

▎ 摘  要

NOVELTY - Preparing graphene oxide-loaded zirconium iron nano-material comprises e.g. (1) dissolving tetrabutyl zirconate in ethanol solution, adding ferric chloride ethanol solution, stirring after finishing dropping; adjusting pH to 8-9 with aqueous ammonia solution, heating to reflux, cooling to room temperature, filtering washing with purified water until no chlorine ions are detected in filtrate, drying to constant weight to obtain zirconium iron nano material precursor; (2) placing the zirconium iron nano material precursor in muffle furnace, calcining, and cooling to room temperature to obtain zirconium iron composite oxide nano material; and (3) ultrasonically dispersing the graphene oxide nanomaterials in purified water, adding zirconium iron composite oxide nanomaterials, carrying ultrasonic treatment, dropwise adding urea aqueous solution to the system, uniformly stirring, transferring to hydrothermal reaction kettle, reacting, cooling to room temperature, filtering. USE - The nano-material is useful for catalyzing organophenols to carry out nitrosation reaction on aromatic ring in presence of nitrates and solvents ( e.g. catalyzing methyl 5-fluoro-2-hydroxybenzoate to prepare methyl 5-fluoro-2-hydroxy-3-nitrobenzoate intermediate drug for treating treatment of ovarian cancer) (all claimed). ADVANTAGE - The method: is environmentally-friendly. DETAILED DESCRIPTION - Preparing graphene oxide-loaded zirconium iron nano-material comprises (1) dissolving tetrabutyl zirconate in ethanol solution, adding ferric chloride ethanol solution, stirring after finishing dropping; adjusting pH to 8-9 with aqueous ammonia solution, heating to reflux for more than 12 hours, cooling to room temperature, filtering washing with purified water until no chlorine ions are detected in filtrate, drying at 70-120 degrees C to constant weight to obtain zirconium iron nano material precursor; where the molar ratio of tetrabutyl zirconate and ferric chloride is 1: 5-8; (2) placing the zirconium iron nano material precursor in muffle furnace, calcining at 500-900 degrees C for 2-5 hours, and cooling to room temperature to obtain zirconium iron composite oxide nano material; and (3) ultrasonically dispersing the 1 g graphene oxide nanomaterials in purified water for 1-2 hours, adding zirconium iron composite oxide nanomaterials, carrying ultrasonic treatment for 2-3 hours, dropwise adding 10 ml urea aqueous solution (20 mmol/l) to the system, uniformly stirring, transferring to hydrothermal reaction kettle, reacting at 140-160 degrees C for 8-12 hours, cooling to room temperature, filtering, washing with purified water and acetone, drying under reduced pressure at 40-80 degrees C to obtain graphene oxide-loaded zirconium iron nano-material. An INDEPENDENT CLAIM is also included for use of graphene oxide-loaded zirconium iron nano-material for catalyzing the organophenols to carry out nitrosation reaction on aromatic ring in the presence of nitrates and solvents.