• 专利标题:   Preparation of comonomer active polymer-modified graphene oxide by preprocessing graphene oxide, reacting with sulfuric acid to obtain functionalized graphene oxide, dissolving in organic solvent, adding into reaction system, and heating.
  • 专利号:   CN105199436-A
  • 发明人:   KANG P, WANG N, WANG S, ZHANG J
  • 专利权人:   UNIV SHENYANG CHEM TECHNOLOGY
  • 国际专利分类:   C08F212/08, C08F220/06, C08K003/04, C08K009/02, C08K009/04, C09C001/46, C09C003/06, C09C003/10
  • 专利详细信息:   CN105199436-A 30 Dec 2015 C09C-001/46 201630 Pages: 7 English
  • 申请详细信息:   CN105199436-A CN10708405 28 Oct 2015
  • 优先权号:   CN10708405

▎ 摘  要

NOVELTY - Preparation of comonomer active polymer-modified graphene oxide includes adding graphite powder into concentrated sulfuric acid, ice-water bath reacting, adding sodium nitrate powder and potassium permanganate, stirring, water bath heating, adding into reaction flask containing deionized water, reacting, adding hydrogen peroxide, vacuum filtering, adding hydrochloric acid, centrifuging, and washing to obtain graphene oxide; adding sulfuric acid, reacting, washing, and vacuum freeze-drying to obtain functionalized graphene oxide; and mixing oil-soluble initiator and organic solvent. USE - Method for preparation of comonomer active polymer-modified graphene oxide (claimed). ADVANTAGE - The method prepares graphene oxide through improved Hummers method and acid treatment, copolymerizes styrene and acryloyl chloride which has good chemical stability, improves dispersibility of graphene oxide in polymer and enables graphene oxide to be more easily dispersed in phenyl ring-containing polymers, and has improved reaction efficiency and reaction extent of graphene oxide grafting, and high efficiency reaction between acryloyl chloride and hydroxyl group. DETAILED DESCRIPTION - Preparation of comonomer active polymer-modified graphene oxide comprises: (A) adding 3-5 g graphite powder into 80-120 mL concentrated sulfuric acid, ice-water bath reacting to 0 degrees C while stirring at speed of 180-300 revolutions/minute (rpm) for 2-4 hours, adding 1-3 g sodium nitrate powder at room temperature, stirring for 1-2 hours, adding 10-25 g potassium permanganate, stirring for 1-2 hours, and water bath heating to 30-50 degrees C for 1-2 hours; and increasing temperature to 90-100 degrees C, gradually adding into reaction flask containing 200-250 mL deionized water, reacting for 1-2 hours, adding 15-20 mL 30% hydrogen peroxide, vacuum filtering, adding 0.1-0.3 mol/L hydrochloric acid, centrifuging, and washing to obtain graphene oxide; (B) adding 0.2-0.5 mol/L sulfuric acid, reacting to 50-70 degrees C while stirring for 3-5 hours, washing, and vacuum freeze-drying to obtain functionalized graphene oxide; and (C) mixing 10-25 mg oil-soluble initiator and 40-70 mL organic solvent under nitrogen atmosphere, stirring at speed of 150-250 rpm, adding 2-5 mL styrene and 2-5 mL acryloyl chloride, and reacting to 50-70 degrees C for 8-12 hours to obtain reaction system; and adding 40-70 mg functionalized graphene oxide to 40-80 mL organic solvent, sonicating for 4-7 hours, pouring into reaction system, adding acid binding agent, adjusting pH to 7-10, heating to 60-80 degrees C for 5-8 hours, washing, and vacuum drying to 30-50 degrees C.