• 专利标题:   Preparing two-dimensional nickel phosphide graphene photocatalytic material useful for photocatalytic hydrogen evolution performance evaluation, comprises e.g. adding concentrated sulfuric acid and joining in round bottom flask, dispersing graphene oxide into water, and placing precursor into boat.
  • 专利号:   CN115920933-A
  • 发明人:   HAO J, LU K
  • 专利权人:   UNIV JIANGXI SCI TECHNOLOGY
  • 国际专利分类:   B01J027/185, B01J037/08, B01J037/28, C01B003/04
  • 专利详细信息:   CN115920933-A 07 Apr 2023 B01J-027/185 202340 Chinese
  • 申请详细信息:   CN115920933-A CN11403187 10 Nov 2022
  • 优先权号:   CN11403187

▎ 摘  要

NOVELTY - Preparing two-dimensional (2D) nickel phosphide graphene photocatalytic material comprises (1) adding concentrated sulfuric acid and joining in the round bottom flask, adding graphite powder, uniformly stirring, slowly adding potassium permanganate to the round bottom flask in an ice bath, placing the round bottom flask into 35℃ water and stirring for 2 hours, washing with deionized water to remove excess acid, obtaining graphite oxide after one week of dialysis, and obtaining graphene oxide (GO) after graphite oxide is fully ultrasonically stripped, (2) dispersing graphene oxide (GO) into deionized water and ultrasonically obtaining for 30 minutes to obtain graphene oxide aqueous solution, and cleaning the sample with deionized water and freeze-drying to obtain nickel hydroxide-graphene precursor, and (3) placing nickel hydroxide-graphene precursor and sodium hypophosphite into porcelain boat by weight ratio of 1:5. USE - The material is useful for photocatalytic hydrogen evolution performance evaluation (claimed). ADVANTAGE - The material: exhibits high catalytic activity, which is conducive to the sustainable development of the environment and energy; has excellent electrical conductivity and excellent photocatalytic performance, high photocatalytic hydrogen evolution efficiency; is economical; has simple production process; is environmentally friendly and easy to recover; and can be recycled. DETAILED DESCRIPTION - Preparing two-dimensional (2D) nickel phosphide graphene photocatalytic material comprises (1) adding concentrated sulfuric acid and joining in the round bottom flask, adding graphite powder, uniformly stirring, slowly adding potassium permanganate to the round bottom flask in an ice bath, placing the round bottom flask into 35℃ water and stirring for 2 hours, slowly continuously adding deionized water to the round bottom flask after the reaction is over, slowly stirring for 10 minutes, adding deionized water and vigorously stirring for 10 minutes, adding 30% hydrogen peroxide solution and continuously stirring for 30 minutes, centrifuging and washing the mixture in the round bottom flask with aqueous hydrogen chloride at a volume ratio of 1:10 to remove metal ions, washing with deionized water to remove excess acid, obtaining graphite oxide after one week of dialysis, and obtaining graphene oxide (GO) after graphite oxide is fully ultrasonically stripped, (2) dispersing graphene oxide (GO) into deionized water and ultrasonically obtaining for 30 minutes to obtain graphene oxide aqueous solution, adding nickel nitrate hexahydrate ultrasonic for 10 minutes, obtaining the first mixed solution after stirring for 20 minutes, adding the second mixed solution containing trisodium citrate and hexamethylenetetramine to the first mixed solution and stirring for 1 hour to obtain the third mixed solution, heating the third mixed solution to 90℃ and vigorously stirring for 10 hours, centrifuging and washing the third mixed solution to collect samples after the temperature of the reaction solution is lowered to room temperature, and cleaning the sample with deionized water and freeze-drying to obtain nickel hydroxide-graphene precursor, and (3) placing nickel hydroxide-graphene precursor and sodium hypophosphite into porcelain boat by weight ratio of 1:5, adopting two-stage calcination method for calcination, and obtaining the 2D nickel phosphide graphene photocatalytic material after the temperature of the tube furnace dropped to room temperature. INDEPENDENT CLAIMS are also included for: 2D nickel phosphide graphene photocatalytic material prepared by the preparation method, where in the X-ray photoelectron spectroscopy of the 2D nickel phosphide graphene photocatalytic material, the peaks at 852.9 eV and 857.14 eV are attributed to Ni 2p3/2, the peak at 874.4eV is attributed to Ni 2p1/2, the peak at 861.2 eV is assigned to the satellite peak of Ni 2p3/2, the peak at the position of 879.1 eV is attributed to the satellite peak of Ni 2p1/2, and the two peaks at 129.9 eV and 134.1 eV correspond to P2p3/2 of metal phosphides and oxidized phosphides; and performance evaluation methods for photocatalytic hydrogen evolution, comprising adding the 2D nickel phosphide graphene photocatalytic material of 1 mg and 15 mg eosin Y in the quartz reactor of 50 ml, adding 5 ml deionized water and 1 ml triethanolamine solution to obtain intermediate mixed solution, introducing 30 minutes argon to make the intermediate mixed solution reach saturation before the reaction starts, and taking 1 ml of gas into the chromatographic detector to detect the hydrogen output after the sample reaction every 2 hours after the start of light.