• 专利标题:   Preparing magnetic graphene complex titania nano-material comprises adding natural graphite and sodium nitrite into three-necked flask at room temperature, cooling under ice bath, adding concentrated sulfuric acid into flask and stirring.
  • 专利号:   CN104857961-A
  • 发明人:   ZHANG Z, HU J
  • 专利权人:   UNIV CHANGZHOU
  • 国际专利分类:   B01J021/06, B01J021/18, B01J023/755, B82Y030/00, B82Y040/00
  • 专利详细信息:   CN104857961-A 26 Aug 2015 B01J-023/755 201614 Pages: 5 Chinese
  • 申请详细信息:   CN104857961-A CN10202183 24 Apr 2015
  • 优先权号:   CN10202183

▎ 摘  要

NOVELTY - Preparing magnetic graphene complex titania nano-material comprises adding natural graphite and sodium nitrite into three-necked flask at room temperature, cooling under ice bath, adding concentrated sulfuric acid into the flask, stirring, adding potassium permanganate, stirring, adding potassium permanganate in three batches, taking out from ice bath, heating and stirring to obtain a brown suspension, adding deionized water, reacting, adding a mixed solution of hydrogen peroxide-ultrapure water to obtain golden graphite oxide dispersion, filtering, washing and drying to yield graphite oxide. USE - The method is useful for preparing magnetic graphene complex titania nano-material (claimed). ADVANTAGE - The nano-material is simple and economical to prepare with controllable reaction conditions and less equipment requirements, has good catalytic performance and can be recycled. DETAILED DESCRIPTION - Preparing magnetic graphene complex titania nano-material comprises: (i) adding 2 g natural graphite and 1 g sodium nitrite into a 250 ml three-necked flask at room temperature, then cooling to 0 degrees C under ice bath, slowly adding 50 ml concentrated sulfuric acid into the three-necked flask, stirring for 30 minutes, adding 0.3 g potassium permanganate, stirring for 30 minutes, adding 7 g potassium permanganate in three batches within 1 hour, taking out from ice bath, heating to 35 plus minus 3 degrees C, stirring for 2 hours to obtain a brown suspension, slowly adding 90 ml deionized water into the three-necked flask, raising temperature to 90 degrees C and reacting for 15 minutes, adding a mixed solution of 7 ml hydrogen peroxide and 55 ml ultrapure water (at 45 degrees C) to obtain golden graphite oxide dispersion, filtering when it is hot, washing to neutrality and drying to yield graphite oxide; (ii) dissolving nickel salt and iron salt (n(Ni2+):n(Fe3+) is 1:2) in deionized water to obtain solution-A, dissolving sodium hydroxide in deionized water to obtain solution-B, drop-wisely adding solution-B into solution-A, stirring vigorously for 20 minutes, then transferring into 100 ml hydrothermal reaction vessel, reacting at 180-220 degrees C for 10-12 hours, cooling naturally, taking out and separating via magnetic field, washing 3 times, drying at 200 degrees C for 4 hours, then grinding to obtain nickel ferrite powder; and (iii) adding proper volume of absolute ethanol into 100 ml beaker at room temperature, drop-wisely adding tetrabutyl titanate under magnetic stirring condition for 10 minutes, then adding acid and stirring for 10 minutes to obtain solution-C, adding proper amount of nickel ferrite powder into deionized water, then adding proper amount of graphite oxide, ultrasonicating for 10 minutes to obtain solution-D, adding solution-D into solution-A, ultrasonicating for 30 minutes, transferring into 100 ml hydrothermal reaction vessel, carrying out hydrothermal reaction at 80-120 degrees C for 18-22 hours, filtering when it is hot, washing, drying and grinding to obtain magnetic titania-graphite oxide photocatalyst powder.