• 专利标题:   Preparing magnetic nanomaterial graphene-rod-shaped ferroferric oxide nanocomposite material comprises e.g. placing black precipitate in water bath to precipitate graphene-ferric oxide precipitate, and washing.
  • 专利号:   CN111747402-A
  • 发明人:   CAI K, OUYANG J, GU J, CAO Y, ZHENG C, ZUO H, LIU S, DENG S, MAO F, XUE Y
  • 专利权人:   HUST TONGJI MEDICAL COLLEGE UNION HOSPIT
  • 国际专利分类:   C01B032/184, C01B032/19, C01G049/06
  • 专利详细信息:   CN111747402-A 09 Oct 2020 C01B-032/184 202088 Pages: 7 Chinese
  • 申请详细信息:   CN111747402-A CN10631724 03 Jul 2020
  • 优先权号:   CN10631724

▎ 摘  要

NOVELTY - Preparing magnetic nanomaterial graphene-rod-shaped ferroferric oxide nanocomposite material comprises e.g. taking graphite powder as raw material to obtain graphene by Hummers method, assembling reaction flask in ice water bath, mixing graphite powder, sodium nitrate and concentrated sulfuric acid, stirring, then adding potassium perchlorate, adding potassium permanganate in batches, adding deionized water gradually, heating, and stirring, adding double brine to reduce residual oxidant, and drying filter cake, crushing filter cake, transferring into a flask, preparing nano ferroferric oxide particles in situ on the graphene nanosheets from iron (III) and iron(II), iron chloride solution and ferrous sulfate heptahydrate, placing black precipitate in water bath at 40-65 degrees C for 15-30 minutes to precipitate graphene-ferric oxide precipitate, and washing mixture repeatedly with deionized water and ethanol 3-5 times. USE - The nanocomposite material is useful in biomedicine, chemical industry, electromagnetic and other fields, targeted therapy, magnetic hyperthermia and other biomedical fields and electromagnetic fields. ADVANTAGE - The nanocomposite material: has high mechanical strength, high surface area, electrical conductivity, in vivo stability, stronger stability and magnetism, and biological safety; and is not easily biodegradable. DETAILED DESCRIPTION - Preparing magnetic nanomaterial graphene-rod-shaped ferroferric oxide nanocomposite material comprises (i) (a) taking graphite powder as raw material to obtain graphene by Hummers method, assembling 500 ml reaction flask in ice water bath, mixing 3-10 g graphite powder, 1-3 g sodium nitrate and 100-120 ml concentrated sulfuric acid uniformly, stirring for 2-5 minutes, then adding 12-18 g potassium perchlorate, (ii) adding 5-10 g potassium permanganate in batches, maintaining temperature at 10-15 degrees C, removing the ice bath, continuously stirring the reaction flask using electromagnetic stirrer for 10-24 hours, adding 150-200 ml deionized water gradually, heating at 70-98 degrees C, and stirring for 10-20 minutes, (iii) adding double brine to reduce residual oxidant after waiting for the color of the solution to change, performing centrifugal separation of graphite suspension at 8000-10000 revolutions/minute, washing to make the pH value greater than or equal to 6 using 2-4% hydrochloride solution, and drying filter cake and allowing to stand, (ii) (a) crushing the filter cake, weighing 150-250 mg and dispersing in 40-50 ml fusion solution to obtain suspension, cooperating with ultrasonic dispersion to obtain stable colloidal suspension after 40-80 minutes, (b) transferring into a flask, adding the compounding solution and heating at 70-80 degrees C, refluxing for 5-8 hours, performing centrifugal separation, placing in DEG solution, performing ultrasonic treatment to obtain graphene solution, (iii) (a) preparing nano ferroferric oxide particles in situ on the graphene nanosheets from iron (III) and iron(II) in a molar ratio of 1.5:1, iron chloride solution and ferrous sulfate heptahydrate, (b) taking ferric chloride, ferrous sulfate and sodium hydroxide solution as raw materials to obtain ferroferric oxide particles, treating above three solutions under ultrasound and adding sodium hydroxide, performing ultrasound treatment for 15-20 minutes to obtain black precipitate, (iii) placing black precipitate in water bath at 40-65 degrees C for 15-30 minutes to precipitate graphene-ferric oxide precipitate, and (iv) washing mixture repeatedly with deionized water and ethanol 3-5 times to obtain graphene-rod-shaped ferroferric oxide nanocomposite.