• 专利标题:   Preparation of magnetic graphene oxide molecularly imprinted composite material for e.g. removing clofibric acid in water involves stirring natural flake graphite in ice-water bath and slowly adding concentrated sulfuric acid.
  • 专利号:   CN104098729-A, CN104098729-B
  • 发明人:   DAI C, ZHANG Y, ZHOU X, LIU Y
  • 专利权人:   UNIV TONGJI
  • 国际专利分类:   B01J020/26, B01J020/30, C02F001/28, C08F212/36, C08J009/26, C08K003/04, C08K003/22
  • 专利详细信息:   CN104098729-A 15 Oct 2014 C08F-212/36 201503 Pages: 12 Chinese
  • 申请详细信息:   CN104098729-A CN10309288 02 Jul 2014
  • 优先权号:   CN10309288

▎ 摘  要

NOVELTY - Magnetic graphene oxide (GO) molecularly imprinted composite material is prepared by stirring natural flake graphite in ice-water bath, slowly adding 150-250 ml concentrated sulfuric acid, maintaining temperature at 0 plus minus 5 degrees C, adding 3-5 g sodium nitrate and 15-30 g potassium permanganate (KMnO4) mixture, controlling reaction temperature at less than or equal to 15-25 degrees C, heating to 30-35 degrees C, stirring in water bath for 15-45 minutes, slowly adding 100-500 ml deionized water, heating to 70-100 degrees C, maintaining temperature for 10-20 minutes, diluting with warm water to 1000-1500 ml, and adding 30% hydrogen peroxide. USE - Preparation of magnetic graphene oxide molecularly imprinted composite material for removing clofibric acid in water and selectively separating trace drug in water system (all claimed). ADVANTAGE - Magnetic GO molecularly imprinted composite material has high efficiency, large surface area, improved regeneration and reuse performance. DETAILED DESCRIPTION - Magnetic graphene oxide (GO) molecularly imprinted composite material is prepared by stirring natural flake graphite in ice-water bath, slowly adding 150-250 ml concentrated sulfuric acid, maintaining temperature at 0 plus minus 5 degrees C, adding 3-5 g sodium nitrate and 15-30 g potassium permanganate (KMnO4) mixture, controlling reaction temperature at less than or equal to 15-25 degrees C, heating to 30-35 degrees C, stirring in water bath for 15-45 minutes, slowly adding 100-500 ml deionized water, heating to 70-100 degrees C, maintaining temperature for 10-20 minutes, diluting with warm water to 1000-1500 ml, adding 100-500 ml 30% hydrogen peroxide solution to remove remaining KMnO4 and turn solution from brown-yellow to bright yellow, centrifuging, washing and centrifuging with anhydrous ethanol, 5% hydrogen chloride (HCl) solution, and deionized water until filtrate does not contain sulfate ions, vacuum-drying in 50 degrees C oven for 48 hours to obtain GO powder, sealing, adding 1-2 g GO powder into flask, adding 150-300 ml dimethylformamide, ultrasonically dispersing for 10-60 minutes, adding 0.5-1.5 g iron(II,III) oxide (Fe3O4), heating to 140-155 degrees C with heating rate of 5-10 degrees C/minute, reacting for 3-5 hours, cooling, separating magnetic GO using permanent magnet, washing with deionized water 3 times, drying for 24 hours in freeze-drier to obtain magnetic GO particles, dissolving 0.1-1.2 mmol template molecule in 20-130 ml pore-forming agent, ultrasonically treating for 10-60 minutes to obtain pre-assembly solution, adding 0.1-10 g magnetic GO particles to 1-10 ml oleic acid, ultrasonically treating for 5-20 minutes, adding 1-10 mmol crosslinker and pre-assembly solution, ultrasonically mixing for 5-60 minutes to obtain pre-polymerization solution, adding 1-10 g dispersant and 100-500 ml pore-forming agent, mixing, adding 0.1-1 g initiator in ice bath, introducing nitrogen for 5-20 minutes to remove oxygen in reactor, sealing, heating to 45-83 degrees C with heating rate of 0.2-0.5 degrees C/minute, performing high-speed rotating reaction for 8-45 hours to obtain molecularly imprinted composite material, placing in methanol:acetic acid solvent with volume ratio of 1-10:10-1, and performing Soxhlet extraction for 10-120 hours to remove template molecule in which template molecule is clofibric acid. DESCRIPTION OF DRAWING(S) - The drawing shows a graph of the hysteresis curve of iron(II,III) oxide, magnetic GO, and molecularly imprinted composite material. (Drawing includes non-English language text).