• 专利标题:   Urea-formaldehyde resin-based method for preparation of graphene oxide adsorption microspheres, involves adding graphite powder, concentrated sulfuric acid, potassium persulfate and phosphorus pentoxide and adding formaldehyde and urea.
  • 专利号:   CN105859992-A, CN105859992-B
  • 发明人:   GUAN P, LIAO Y, YANG Y, CHE Y, XIAO S
  • 专利权人:   UNIV CENT SOUTH FORESTRY TECHNOLOGY, HUNAN JINPAN NEW MATERIAL TECHNOLOGY CO
  • 国际专利分类:   C01B031/04, C08G012/12, C08J003/12, C08K003/04, C08L061/24, C01B032/198
  • 专利详细信息:   CN105859992-A 17 Aug 2016 C08G-012/12 201672 Pages: 7 Chinese
  • 申请详细信息:   CN105859992-A CN10198544 01 Apr 2016
  • 优先权号:   CN10198544

▎ 摘  要

NOVELTY - The urea-formaldehyde resin-based method for preparation of graphene oxide adsorption microspheres, involves adding graphite powder, concentrated sulfuric acid, potassium persulfate and phosphorus pentoxide, adding concentrated sulfuric acid, sodium nitrate and potassium permanganate, adding hydrogen peroxide, dispersing graphene oxide in water, adding formaldehyde and urea, cooling to room temperature to obtain graphene oxide/urea resin composite material, carrying out atomizing treatment, spraying atomized material in curing agent, curing to obtain final product. USE - Urea-formaldehyde resin-based method for preparation of graphene oxide adsorption microspheres (claimed). ADVANTAGE - The urea-formaldehyde resin-based method enables preparation of graphene oxide adsorption microspheres with uniform particle size, excellent stability, rich oxygen-containing functional groups on the composite material, large pore diameter and uniform distribution of pore channels and excellent chelating ability. DETAILED DESCRIPTION - Urea-formaldehyde resin-based method for preparation of graphene oxide adsorption microspheres, involves adding 1-3 pts. wt. graphite powder, 95-98% of 50-150 pts. wt. concentrated sulfuric acid, 1-3 pts. wt. potassium persulfate and 1-3 pts. wt. phosphorus pentoxide and uniformly mixing in a sealed reaction vessel, stirring evenly under the condition of ice bath, heating at 60-100 degrees C in water bath under heating condition, stirring and reacting for 6-12 hours under reduced pressure, filtering, washing, drying the filtrate under vacuum, grinding, adding 95-98% of 100-200 pts. wt. concentrated sulfuric acid and 1-2 pts. wt. sodium nitrate and 7-11 pts. wt. potassium permanganate, reacting for 1-3 hours under the condition of ice bath, heating at 30-70 degrees C for 46-52 hours, adding 8-12% of 10-40 pts. wt. hydrogen peroxide, maintaining the reaction under the condition of ice bath for 2-4 hours, cooling to room temperature to obtain suspension, carrying out centrifugal sedimentation process, removing supernatant, adding sediment to deionized water, stirring, carrying out centrifugal sedimentation process, removing supernatant, adding sediment to anhydrous ethanol, stirring, carrying out centrifugal sedimentation process, washing the sediment with anhydrous ethanol, drying the precipitate under vacuum to obtain the graphene oxide, uniformly dispersing graphene oxide in water to obtain graphene oxide aqueous solution, adding formaldehyde and urea in molar ratio of 1.2:1, adding certain amount of formaldehyde solution, adjusting pH to alkaline using sodium hydroxide solution, stirring for 10-30 minutes, adding urea batch (I), heating at 80-100 degrees C for 40-60 minutes, adjusting pH to acidic using ammonium chloride solution, adding urea batch (II) and aqueous solution of graphene oxide, heating at 80-100 degrees C for 30-50 minutes, adjusting pH to alkaline using sodium hydroxide solution, adding urea batch (III), heating at 40-80 degrees C for 20-40 minutes, cooling to room temperature to obtain graphene oxide/urea resin composite material, carrying out atomizing treatment of composite material using high pressure spray gun, spraying atomized material in curing agent for molding, curing, vacuum filtering and washing with water to obtain micron-sized graphene oxide adsorption microspheres. The amount of urea batch (I) in total urea is 35-45 wt.%. The amount of urea batch (II) in total urea is 35-45 wt.%. The amount graphene oxide in total amount of urea is 0.5-1.5 wt.% The amount of urea batch (III) in total urea is 10-30 wt.%.