• 专利标题:   Degrading highly efficient methylene blue comprises e.g. preparing methylene blue aqueous solution, then adding into reaction tube and ultrasonically dispersing graphene/titania hollow composite microspheres in methylene blue.
  • 专利号:   CN107486110-A, CN107486110-B
  • 发明人:   XIA W, ZHOU W, ZHANG Y, XIAO W
  • 专利权人:   UNIV CHONGQING ARTS SCI, UNIV CHONGQING ARTS SCI
  • 国际专利分类:   B01J013/02, B01J021/18, B01J035/08, C02F001/32, C02F001/72, C02F101/30
  • 专利详细信息:   CN107486110-A 19 Dec 2017 B01J-013/02 201806 Pages: 9 Chinese
  • 申请详细信息:   CN107486110-A CN10872894 20 Jul 2015
  • 优先权号:   CN10425962, CN10872894

▎ 摘  要

NOVELTY - Degrading highly efficient methylene blue comprises e.g. (i) preparing methylene blue aqueous solution at a concentration of 10 mg/l and adding 48 ml to reaction tube, then ultrasonically dispersing 5 mg graphene/titania hollow composite microspheres in 2 ml methylene blue having concentration of 10 mg/l aqueous solution, then adding to reaction tube under stirring, (ii) placing reaction tube obtained in (i) in a photochemical reactor, high-pressure mercury lamp is used as an ultraviolet light source, then setting power to 300 W, and performing photocatalytic reaction under vigorous stirring. USE - The method is useful for degrading highly efficient methylene blue (claimed). DETAILED DESCRIPTION - Degrading highly efficient methylene blue comprises (i) preparing methylene blue aqueous solution with a concentration of 10 mg/l, adding 48 ml into reaction tube, then ultrasonically dispersing 5 mg graphene/titanium dioxide hollow composite microspheres in 2 ml methylene blue aqueous solution having concentration of 10 mg/l, adding dropwise to the above reaction tube with stirring; and the preparation of graphene/titanium dioxide hollow composite microspheres includes (a) preparing mono0dispersed silica colloidal microspheres with controlled size, where the particle size of silica colloidal microspheres is 200-500 nm, (b) electrostatic effect on the surface of the silica microspheres assembly of a layer of cationic polyelectrolyte poly(acrylamide-co-diallyldimethylammonium chloride), and the surface of the silica microspheres is positively electrified, (c) ultrasonic-assisted self-assembly method of the small-sized graphene oxide coated on the silica microsphere surface, the size of the small size of graphene oxide film does not exceed the radial size of 200nm, so as to prepare silica/graphene composite microspheres with good water dispersibility; the self-assembly method is to self-assemble the small-size graphene oxide sheet with negative surface by electrostatic action on the surface of the positively-charged surface of silica microsphere in (ii) under continuous intense ultrasonic conditions, (d) ultrasonically dispersing silica/graphene composite microspheres in water, adding into anhydrous ethanol under sonication conditions, then adding polyvinylpyrrolidone solution, stirring at room temperature for 30 minutes and then adding titanium tetrafluoride aqueous solution and stirring to form reaction system; the total volume ratio between ethanol and water in the reaction system is 5:2, the mass ratio of silica/graphene oxide composite microspheres and titanium tetrafluoride is 2:5, the average molecular weight of polyvinylpyrrolidone is 40,000 and the concentration is 20 mg/ml, (e) transferring reaction system to the reactor, carrying out the reaction at 180 degrees C, performing solvothermal for 4 hours, cooling, separating the precipitate by centrifugation, washing with water many times and then vacuum drying; and (ii) placing reaction tube in step (i) in a photochemical reactor, high-pressure mercury lamp used as an ultraviolet light source, then setting the power to 300 and performing photocatalytic reaction under vigorous stirring.