• 专利标题:   Preparing phosphorus-sulfur co-doped graphene-supported molybdenum carbide composite material in electrochemical synthesis of ammonia by adding graphene oxide to deionized water, ultrasonically dispersing, transferring to muffle furnace, adding ammonium molybdate solution, and passing hydrogen.
  • 专利号:   CN113005477-A, CN113005477-B
  • 发明人:   FENG K
  • 专利权人:   HANGZHOU GUORAN TRADING CO LTD, BEIJING TIME STONE TECHNOLOGY CO LTD
  • 国际专利分类:   C25B001/27, C25B011/091
  • 专利详细信息:   CN113005477-A 22 Jun 2021 C25B-011/091 202168 Pages: 9 Chinese
  • 申请详细信息:   CN113005477-A CN10213147 26 Feb 2021
  • 优先权号:   CN10213147

▎ 摘  要

NOVELTY - Method for preparing phosphorus-sulfur co-doped graphene-supported molybdenum carbide composite material involves (a) adding graphene oxide to deionized water, ultrasonically dispersing, adding phosphoric acid, ultrasonically mixing, pouring the mixed sample into a watch glass, placing in a drying oven to dry, and transferring to a muffle furnace, (b) adding the product of step (a) to deionized water, ultrasonically dispersing, and ultrasonically adding sulfuric acid to mix uniformly, freeze-drying, followed by calcination reaction, (c) adding the product of step (b) to deionized water, adding ammonium molybdate tetrahydrate into deionized water, dripping ammonium molybdate solution to phosphorus-sulfur co-doped graphene solution, rinsing the product with deionized water and ethanol, drying in vacuum, placing the product in a tube furnace, passing hydrogen first, and calcining in hydrogen atmosphere to obtain the product. USE - The method is used for preparing a phosphorus-sulfur co-doped graphene-supported molybdenum carbide composite material which is used in electrochemical synthesis of ammonia (claimed), and for electrocatalytic nitrogen reduction. ADVANTAGE - The material prepared by the method has excellent catalytic performance, and has a good market prospect. DETAILED DESCRIPTION - Method for preparing phosphorus-sulfur co-doped graphene-supported molybdenum carbide composite material involves (a) adding graphene oxide to deionized water, ultrasonically dispersing for 1 hour, adding phosphoric acid, ultrasonically mixing for 8 hours uniformly, pouring the mixed sample into watch glass, placing in a drying oven to dry, and transferring to a muffle furnace for calcination reaction, (b) adding the product of step (a) to deionized water, ultrasonically dispersing for 1 hour, and ultrasonically adding sulfuric acid for 2 hours to mix uniformly, freeze-drying, followed by calcination reaction to obtain phosphorus-sulfur co-doped graphene material, (c) adding the product of step (b) to deionized water, ultrasonically obtaining completely dispersed, adding ammonium molybdate tetrahydrate to deionized water, stirring to make completely dissolved, dripping ammonium molybdate solution to phosphorus-sulfur co-doped graphene solution, and stirring for 10-12 hours, rinsing the product with deionized water and ethanol, drying in vacuum, placing the product in a tube furnace, passing hydrogen first, exhausting the gas inside the tube furnace, and calcining in an hydrogen atmosphere to obtain the product.