• 专利标题:   Preparing silver-loaded magnetic graphene-based titanium dioxide nanotube complex material comprises e.g. preparing magnetic graphene oxide, titanium dioxide nanotube and silver loaded titanium dioxide.
  • 专利号:   CN105771978-A
  • 发明人:   LI J, LUO C, WANG X, WANG Y, SUN Y, DUAN H, DING C
  • 专利权人:   UNIV JINAN
  • 国际专利分类:   B01J023/50, C02F001/30
  • 专利详细信息:   CN105771978-A 20 Jul 2016 B01J-023/50 201683 Pages: 8 Chinese
  • 申请详细信息:   CN105771978-A CN10162248 22 Mar 2016
  • 优先权号:   CN10162248

▎ 摘  要

NOVELTY - Preparing silver-loaded magnetic graphene-based titanium dioxide nanotube complex material comprises e.g. adding graphene oxide, anhydrous ferric trichloride and ferrous chloride with water and aqueous ammonia mixture, heating, separating, washing, drying, dispersing P25 titanium dioxide powder in sodium hydroxide solution, mixing, incubating, centrifuging, washing, centrifuging, drying, dispersing magnetic graphite oxide and silver loaded titanium dioxide nanotubes with deionized water, reacting, centrifuging, washing and drying. USE - The method is useful for preparing silver-loaded magnetic graphene-based titanium dioxide nanotube complex material (claimed). ADVANTAGE - The method has visible light degradation efficiency as high as 95%, has easy separation and easy recovery. DETAILED DESCRIPTION - Preparing silver-loaded magnetic graphene-based titanium dioxide nanotube complex material comprises (a) preparing magnetic graphene oxide by taking graphene oxide, anhydrous ferric trichloride and ferrous chloride in a mass ratio of 5:5:3:2:2:1 (proportion maximum 4-8 times), adding a mixture of ultra-pure water under nitrogen gas protection, mechanically stirring at 90 degrees C while stirring, adding aqueous ammonia with a pH value of 8-10 in a dropwise manner, heating while stirring for 0.5-1 hours, cooling, magnetic suction separating, washing with ethanol for two times, placing in a vacuum drying box and drying, (b) preparing titanium dioxide nanotube by ultrasonically dispersing 0.3-1 g P25 titanium dioxide powder in 60 ml sodium hydroxide solution (6-10 mol/l) for 0.5-1 hour, dark mixing for 10-12 hours, transferring to a PTFE-lined stainless steel hydrothermal reactor, sealing, placing in the drying oven, heating at 120-150 degrees C (maximum of not greater than 150 degrees C), incubating for 36-48 hours, naturally cooling, separating by centrifuging, washing the samples with ultrapure water until neutral, repeatedly washing with 0.01-0.1 mol/l hydrochloric acid solution to a pH close to the pH of the hydrochloric acid solution, repeatedly cleaning with ultra-pure water, washing out the aqueous solution until the pH is close to neutral, centrifuging, drying at 50-80 degrees C for 8-12 hours, to obtain titanate nanotubes, calcining at 400-450 degrees C (the maximum of not greater than 450 degrees C), to obtain calcined titanium dioxide nanotubes, (c) preparing silver loaded titanium dioxide nanotubes by adding titanium dioxide nanotubes and silver nitrate to the aqueous solution (0.1-2% silver/titanium material), ultrasonically dispersing for 10-30 minutes, stirring for 8-12 hours, centrifuging the samples, washing for three times with deionized water, drying at 100 degrees C, to obtain silver loaded titanium dioxide nanotubes, roasting the solid powder in a muffle furnace at 450-500 degrees C for 1-2 hours, to obtain silver loaded titanium dioxide nanotubes, (d) preparing silver-loaded magnetic graphene-based titanium dioxide nanotube complex comprising taking magnetic graphite oxide and silver loaded titanium dioxide nanotubes in a mass ratio of 1:5-3:7, adding deionized water, ultrasonically dispersing for 0.5-1 hours, stirring, transferring to a hydrothermal reaction kettle to carry out hydrothermal reaction for 1-3 hours at 100-120 degrees C, cooling, removing the reaction solution, centrifuging, thoroughly washing with deionized water, to obtain a solid precipitate and drying at 50 degrees C. An INDEPENDENT CLAIM is also included for the catalytic degradation of the silver-loaded magnetic graphene-based titanium dioxide nanotube complex material comprising carrying out photocatalytic reaction in the light box and determining by an UV spectrophotometer including (a) pre-treating test solution by taking 0.0050 g plasticizer (dioctyl phthalate), dissolving in 250 mL volumetric flask (20.00 mg/l solution of dioctyl phthalate) and shaking, transferring 50 ml into a 100 ml beaker, adjusting the pH to 4, taking 0.0150 g silver loaded magnetic graphene-based titanium dioxide nanotube complex into the beaker and evenly shaking, to form uniform test solution, (b) photocatalytic degradation by placing beaker containing 50 ml test solution in a photocatalytic reaction tank, stirring in a dark room for 20 minutes, removing the supernatant, irradiating with UV light (the current size of 15 A), taking supernatant once in every five minutes (sample 4 ml), taking distilled water as the reference solution in the UV spectrophotometer, measuring the absorbance values A of the solutions before and after the degradation in the wavelength range of 200-800 nm, calculating the degradation rate by calculating the degradation efficiency with reference to the following formula as eta is equal to 100%, where A0 and As are respectively absorbance value of before degradation and after degradation time t of plasticizer (dioctyl phthalate) solution and eta is the rate of degradation under certain conditions.