• 专利标题:   Preparing core-shell graphene oxide/silver composite material by dispersing aminated surface modified silver particles in water, and mixing e.g. surface modified graphene oxide and 1-ethyl-(3-dimethylamino propyl) carbodiimide hydrochloride.
  • 专利号:   CN104399415-A, CN104399415-B
  • 发明人:   CHANG L, ZHAO Y, CHEN S
  • 专利权人:   UNIV JILIN NORMAL
  • 国际专利分类:   B01J013/02, B01J031/26
  • 专利详细信息:   CN104399415-A 11 Mar 2015 B01J-013/02 201533 Pages: 12 Chinese
  • 申请详细信息:   CN104399415-A CN10531162 09 Oct 2014
  • 优先权号:   CN10531162

▎ 摘  要

NOVELTY - Preparation of core-shell graphene oxide/silver composite material comprises preparing pre-oxidizing graphite powders; preparing graphene oxide with controllable size; preparing surface modified graphene oxide sheet; preparing silver particle; preparing aminated surface of modified silver particles; and taking aminated surface of modified silver particles, dispersing in ultra-pure water, dispersing, taking surface modified graphene oxide, dispersing in pure water, dispersing, mixing 1-ethyl-(3-dimethylamino propyl) carbodiimide hydrochloride and N-hydroxy succinimide, reacting, and drying. USE - Method for preparing core-shell graphene oxide/silver composite material (claimed). ADVANTAGE - The simple and green method produces material with 532 nm excitation wavelength, good surface enhanced Raman scattering, and good application prospect in water environment treatment field and biological detection. DETAILED DESCRIPTION - Preparation of core-shell graphene oxide/silver composite material comprises preparing pre-oxidizing graphite powders by mixing 10 g potassium persulfate and phosphorus pentoxide at ratio of 1:1-1:10, adding 5-50 ml concentrated sulfuric acid, adding 30 g graphite powders of 30, stirring, reacting at 50-90 degrees c under oil bath for 48 hours, taking out, superpure water washing until neutral, filtering, drying at room temperature for 24 hours; preparing graphene oxide with controllable size by taking 10 g pre-oxidized graphite powder, adding 2-200 ml concentrated sulfuric acid in ice bath for 20 minutes, stirring, slowly adding 6 g potassium permanganate, continuously reacting for 2-20 hours, moving under oil bath at 35 degrees c, magnetic stirring for 2-48 hours, adding 10-1000 ml super-pure water, reacting at 98 degrees C for 15-240 minutes, stirring, cooling to room temperature, adding 20 ml hydrogen peroxide solution, filtering, washing controllable graphene oxide with diluted hydrochloric acid, removing impurity, washing using super-pure water repeatedly, filtering until neutral and drying; preparing surface modified graphene oxide sheet by taking 50-500 mg controllable size graphene oxide, placing 5-500 ml superpure water, ultrasonic dispersing for 4 hours, adding 5-10 g solid sodium hydroxide, dissolving, adding 5-10 g hypochlorite, ultrasonic dissolving using ultrasonic machine for 24 hours, washing with ethanol until neutral and vacuum drying; preparing silver particle by mixing 1 M nitric acid silver and polyvinylpyrrolidone solution, adding 10-100 ml super-pure water, magnetic stirring under room temperature for 10 minutes, adding 1 ml 1 M ascorbic acid solution, rapid stirring for 15 minutes, stopping reaction, separating silver particle and vacuum drying; preparing aminated surface of modified silver particles by taking 0.5-3 g silver particles, dispersing in 1-200 ml ethanol and ultrapure water, adding 0.5-10 ml silane reagent under nitrogen protection and reacting at room temperature for 24 hours; and taking 30-100 mg aminated surface of modified silver particles, dispersing in 40-100 ml ultra-pure water, ultrasonically dispersing for 30 minutes, taking 5-50 mg surface modified graphene oxide, dispersing in 6-200 ml pure water, dispersing for 2 hours, mixing 1-ethyl-(3-dimethylamino propyl) carbodiimide hydrochloride and N-hydroxy succinimide, reacting for 1-48 hours, washing using water, and vacuum drying.