• 专利标题:   Preparing gold/ferroferric oxide/graphene nanohybrid material by ultrasonically mixing oxidized graphene aqueous solution, sodium hydroxide and monochloroacetic acid, reacting, using diluted hydrochloric acid solution and centrifuging.
  • 专利号:   CN107159259-A
  • 发明人:   LU X, WEI H, ZHANG D, ZHANG X, ZHANG S, SHANG D, ZHANG Z
  • 专利权人:   UNIV NORTHWEST NORMAL
  • 国际专利分类:   B01J023/89
  • 专利详细信息:   CN107159259-A 15 Sep 2017 B01J-023/89 201773 Pages: 19 Chinese
  • 申请详细信息:   CN107159259-A CN10344153 16 May 2017
  • 优先权号:   CN10344153

▎ 摘  要

NOVELTY - A gold/ferroferric oxide/graphene nanohybrid material is prepared by ultrasonically mixing oxidized graphene aqueous solution, sodium hydroxide and monochloroacetic acid, reacting, using diluted hydrochloric acid solution, centrifuging, and washing; and dissolving azanine-polyethylene glycol-azanine (H2N-PEG-H2N) (MPEG=6000) in mixed solution of dichloromethane and absolute ethanol, adding 3,4-dihydroxybenzaldehyde, stirring, reacting, adding sodium borohydride, stirring, filtering, vacuum distilling, separating precipitate with ether, washing, and filtering and drying. USE - Method for preparing gold/ferroferric oxide/graphene nanohybrid material (claimed). ADVANTAGE - The material has excellent catalytic performance and visualized detection of heavy metal ion resistance. DETAILED DESCRIPTION - A gold/ferroferric oxide/graphene nanohybrid material is prepared by: (A) ultrasonically mixing 0.02-0.025 pt. wt. of 4.05-4.15 mg/ml oxidized graphene aqueous solution, 2.5-2.7 pts. wt. sodium hydroxide and 2.2-2.23 pts. wt. monochloroacetic acid, reacting for 6 hours to obtain black solution, using diluted hydrochloric acid solution to pH value of 5-6, centrifuging, and washing to obtain carboxyl oxide graphene; (B) dissolving 2.0-3.0 pts. wt. azanine-polyethylene glycol-azanine (H2N-PEG-H2N) (MPEG=6000) in mixed solution of 39.75-45 pts. wt. dichloromethane and 23.67-38 pts. wt. absolute ethanol, adding 0.050-0.54 pt. wt. 3,4-dihydroxybenzaldehyde under ice bath condition, stirring at room temperature, reacting for 36 hours, adding 40.016-0.01858 pt. wt. sodium borohydride, stirring to react at room temperature for 4 hours, filtering, vacuum distilling, separating precipitate with ether, washing, and filtering and drying to obtain H2N-PEG-DIB; (C) adding 0.1-0.015 pt. wt. graphene oxide-carboxylic acid (GO-COOH) into flask, adding 6.6-8.8 pts. wt. dimethyl sulfoxide, ultrasonically dispersing, adding 0.040-0.050 pt. wt. N-ethoxycarbonyl-2-ethoxy-1,2-dihydroquinoline (EEDQ) and 0.040-0.55 pt. wt. H2N-PEG-DIB under magnetic force stirring, continuously reacting for 8 hours, adding 0.0009586-0.0015 pt. wt. diethylenetriamine, continuously stirring and reacting for 48 hours and washing to obtain DETA/PEG/GO; (D) dissolving 0.706-0.708 pt. wt. iron acetylacetonate in benzyl ether and amine mixed solvent of 1:1, reacting at 120 degrees C for 2 hours, sealing nitrogen atmosphere, cooling to room temperature, using anhydrous alcohol, and centrifuging and separating to obtain iron oxide nanoparticles; (E) ultrasonically and uniformly dispersing 0.01-0.015 pt. wt. DETA/PEG/GO in 223.5-250.0 pts. wt. chloroform, stirring at room temperature, dissolving 0.005-0.008 pt. wt. chloroauric acid with 31.56 pts. wt. ethanol, adjusting pH value to 6-7, adding ethanol solution of chloroauric acid to DETA/PEG/GO system, stirring at room temperature for 2 hours, dripping 0.002 g/ml ethanol solution of sodium borohydride, adding 0.010 pt. wt. sodium borohydride, stirring and reacting for 4 hours, rotary steaming at 45 degrees C at 0.06 MPa, spinning solvent, centrifuging, and washing; and (F) transferring into round flask, adding 223.5-250.5 pts. wt. chloroform, ultrasonically and uniformly dispersing, adding 0.001755-0.00351 pt. wt. iron oxide nanoparticle with chloroform to dissolve, slowly dropwise adding into solution with burette, stirring overnight, evaporating, rotary steaming at 45 degrees C at 0.06 MPa, centrifuging, washing, and dispersing in water. The mol ratio of iron acetylacetonate and dibenzyl ether is 1:26.