• 专利标题:   Preparation of nanofiber material used in catalytic degradation of nitrogen oxide, involves reacting e.g. graphene oxide and surface-modified carbonitride nanospheres, and spinning mixture of obtained material and polymer solution.
  • 专利号:   CN105498821-A, US2017173571-A1, CN105498821-B
  • 发明人:   LU J, CHEN D, WU H
  • 专利权人:   UNIV SOOCHOW, UNIV SOOCHOW
  • 国际专利分类:   B01D053/56, B01D053/86, B01J027/24, B01J035/06, B01J021/18, B01J031/06, B01J035/00, B01J035/08, B01J037/00, B01J037/02, B01J037/04, B01J037/08
  • 专利详细信息:   CN105498821-A 20 Apr 2016 B01J-027/24 201656 Pages: 10 English
  • 申请详细信息:   CN105498821-A CN10955976 17 Dec 2015
  • 优先权号:   CN10955976

▎ 摘  要

NOVELTY - Preparation of nanofiber material involves adding an aqueous solution of graphene oxide to an aqueous suspension of surface-modified hollow graphite-phase carbonitride nanospheres, stirring, adding hydrazine hydrate, reacting, centrifuging, washing, drying, obtaining hollow graphite-phase carbonitride nanosphere/reduction-oxidation graphene composite material, adding composite material to polymer dimethylformamide solution, stirring, electrostatically spinning resultant solution, and calcining obtained nanofiber under an inert gas atmosphere. USE - Preparation of hollow graphite-phase carbonitride nanosphere/reduction-oxidation graphene composite material and polymer carbide nanofiber material used in catalytic degradation of nitrogen oxide e.g. nitrogen monoxide (all claimed). ADVANTAGE - The method enables economical preparation of hollow graphite-phase carbonitride nanosphere/reduction-oxidation graphene composite material and polymer carbide nanofiber material with high ppb-level nitrogen oxide adsorption efficiency and excellent repeatability, by simple process. DETAILED DESCRIPTION - Preparation of hollow graphite-phase carbonitride nanosphere/reduction-oxidation graphene composite material and polymer carbide nanofiber material involves adding an aqueous solution of graphene oxide to an aqueous suspension of surface-modified hollow graphite-phase carbonitride nanospheres, stirring at room temperature for 1-2 hours, adding hydrazine hydrate, reacting at 95 degrees C for 1-2 hours, centrifuging, washing, drying, obtaining hollow graphite-phase carbonitride nanosphere/reduction-oxidation graphene composite material, adding composite material to polymer dimethylformamide solution, stirring at room temperature for 5-8 hours, electrostatically spinning resultant solution, and calcining obtained nanofiber at 500-520 degrees C for 4-5 hours under an inert gas atmosphere. The mass ratio of surface-modified hollow graphite-phase carbonitride nanospheres and graphene oxide is 1:0.1-0.3. The mass ratio of graphene oxide and hydrazine hydrate is 1:1-2. The mass ratio of composite material and polymer is 1:15-20. The surface-modified hollow graphite-phase carbonitride nanospheres are prepared by adding 3-aminopropyltriethoxysilane to toluene suspension of hollow graphite-phase carbonitride nanospheres, heating at reflux for 20-24 hours, centrifuging, washing, and drying. The content ratio of hollow graphite-phase carbonitride nanospheres and 3-aminopropyltriethoxysilane is 1 g:3-5 mL. The hollow graphite-phase carbonitride nanospheres are prepared by mixing silica nanospheres and cyanamide in mass ratio of 1:3-7 for 3-5 hours under vacuum condition, ultrasonically processing for 2-3 hours, reacting at 60-70 degrees C for 10-12 hours, centrifuging, calcining obtained solid at 550-570 degrees C for 4-5 hours under an inert gas atmosphere, etching obtained powder using 4M ammonium bifluoride to remove silica nanospheres, centrifuging, washing, and drying. The silica nanospheres are prepared by adding tetraethyl orthosilicate to concentrated aqueous ammonia, adding mixture of ethanol and water, mixing, aging for 1-2 hours, adding mixture of tetraethylorthosilicate and octadecyltrimethoxysilane in mass ratio of 1:1-2, mixing, aging 3-5 hours, centrifuging, drying, calcining at 550-570 degrees C for 6-8 hours, washing calcined product with 1M hydrochloric acid, and drying. The mass ratio of concentrated aqueous ammonia, ethanol, water and tetraethylorthosilicate is 1:15-20:1-5:1-2. The graphene oxide is prepared b adding graphite to concentrated sulfuric acid under ice-cooling and stirring conditions, stirring, adding potassium permanganate with graphite and potassium mass ratio of 1:5-8, reacting at 35-40 degrees C for 15-20 hours, adding reaction mixture to ice-water containing hydrogen peroxide, centrifuging, washing, and drying. The content ratio of graphite and concentrated sulfuric acid is 1 g:20-25 mL.