• 专利标题:   Preparing vanadium phosphate sodium oxide/graphene composite material comprises stirring e.g. sodium salt, vanadium salt, citric acid and deionized water, drying, grinding, dispersing, adding graphene oxide solution and freeze-drying.
  • 专利号:   CN104078676-A, CN104078676-B
  • 发明人:   REN M, LIU W, ZHAO D, ZHOU G
  • 专利权人:   UNIV QILU TECHNOLOGY
  • 国际专利分类:   C01B025/45, H01M004/58
  • 专利详细信息:   CN104078676-A 01 Oct 2014 H01M-004/58 201501 Pages: 8 Chinese
  • 申请详细信息:   CN104078676-A CN10363701 29 Jul 2014
  • 优先权号:   CN10363701

▎ 摘  要

NOVELTY - Preparing vanadium phosphate sodium oxide/graphene composite material comprises stirring sodium salt, vanadium salt, phosphate, oxalic acid, citric acid and deionized water, drying the solution to obtain a gel, heating in an air atmosphere, cooling to room temperature, grinding uniformly, heating in an air atmosphere, grinding, adding deionized water to the obtained powder, ultrasonically dispersing, adding graphene oxide solution, stirring, freeze-drying, adding N-methylpyrrolidone solid powder, dispersing to obtain stable homogeneous dispersion, reacting under microwave and drying. USE - The method is useful for preparing vanadium phosphate sodium oxide/graphene composite material (claimed). ADVANTAGE - The composite material has uniform particles, high electronic conductivity, and excellent electrochemical sodium reservoir performance; and is prepared in simple, cost effective and environmental friendly manner. DETAILED DESCRIPTION - Preparing vanadium phosphate sodium oxide/graphene composite material, comprises: (a) stirring sodium salt, vanadium salt, phosphate, oxalic acid, citric acid and deionized water in a molar ratio of 1:1:1:1-3:200-1000 at 50-90 degrees C for 2-6 hours to obtain a uniform solution, drying the obtained solution at 60-150 degrees C to obtain a gel, where the sodium salt is at least one of sodium carbonate, sodium acetate or sodium dihydrogen phosphate, the vanadium salt is vanadium pentoxide, ammonium metavanadate, vanadium dioxide or vanadium trioxide, and the phosphate is phosphoric acid, ammonium phosphate, ammonium dihydrogen phosphate, sodium dihydrogen phosphate or diammonium phosphate; (b) heating the obtained gel in an air atmosphere to 250-300 degrees C, at a heating rate of 3-10 degrees C/minute for 3-6 hours, cooling to room temperature, grinding uniformly, and heating in an air atmosphere at a heating at a heating rate of 3-10 degrees C/minute to 450-550 degrees C for 3-5 hours, cooling to room temperature, and grinding uniformly to obtain vanadyl sodium phosphate powder; (c) adding deionized water to the obtained powder, ultrasonically dispersing for 1-2 hours to obtain 2-10 mg/ml sodium vanadium phosphate oxygen dispersion, (d) adding graphene oxide into deionized water, ultrasonically dispersing for 2-6 hours to obtain 0.1-2 mg/ml graphene oxide solution, adding the dispersion obtained in the step (c), stirring for 3-6 hours, and freeze-drying to obtain graphene oxide powder having solid content of 5-10 wt.%; and (e) adding N-methylpyrrolidone to the obtained solid powder, dispersing to obtain 10-50 mg/ml stable homogeneous dispersion, reacting under microwave for 2-3 minutes at 60-150 degrees C, and completely drying.