• 专利标题:   Preparation of allyl acetoacetate functionalized graphene oxide used as cadmium ion adsorbent, by adding natural crystalline flake graphite into beaker, placing into water bath, adding concentrated sulfuric acid and continuously stirring.
  • 专利号:   CN106944003-A
  • 发明人:   ZHOU J
  • 专利权人:   JIAXING DEYANG BIOTECHNOLOGY CO LTD
  • 国际专利分类:   B01J020/22, B01J020/30, C02F001/28, C02F101/20
  • 专利详细信息:   CN106944003-A 14 Jul 2017 B01J-020/22 201766 Pages: 8 Chinese
  • 申请详细信息:   CN106944003-A CN10246380 15 Apr 2017
  • 优先权号:   CN10246380

▎ 摘  要

NOVELTY - An allyl acetoacetate functionalized graphene oxide is prepared by adding natural crystalline flake graphite into beaker, placing into water bath filled with ice water mixture, slowly adding concentrated sulfuric acid into beaker, continuously stirring, adding potassium permanganate powder into beaker, stirring, and continuously stirring to obtain reaction liquid 1; and slowly adding deionized water, keeping beaker temperature, continuously stirring, dripping hydrogen peroxide solution, and continuously stirring to obtain bright yellow reaction liquid 2. USE - Method for preparing allyl acetoacetate functionalized graphene oxide used as cadmium ion adsorbent (claimed) in chlor-alkali manufacturing process, papermaking wastewater, oil refining, painting, pharmacy and battery manufacturing industrial production wastewater containing cadmium ions. ADVANTAGE - The product has good economical efficiency and simple preparation technique. DETAILED DESCRIPTION - An allyl acetoacetate functionalized graphene oxide is prepared by: (A) adding 2-2.5 g natural crystalline flake graphite into 1000 mL beaker, placing into water bath filled with ice water mixture, slowly adding 70-100 mL concentrated sulfuric acid into beaker, continuously stirring for 0.5 hour, adding 9.5-13 g potassium permanganate powder into beaker, stirring for 2 hours, and continuously stirring for 24 hours to obtain reaction liquid 1; (B) slowly adding 150-200 mL deionized water, keeping beaker temperature, continuously stirring at 25 degrees C for 0.8 hour, dripping 100-180 mL of 30% hydrogen peroxide solution, and continuously stirring for 0.5 hour to obtain bright yellow reaction liquid 2; (C) placing into centrifugal tube, high speed centrifuging for 20 minutes at speed of 10000 revolutions/minute (rpm), removing supernatant, washing precipitated solid with 20 mL of 5% hydrochloric acid solution, centrifuging for 20 minutes at speed of 7000 rpm, removing supernatant, leaving precipitated solid, washing with 5% hydrochloric acid for 3 times, adding precipitate with 100 mL deionized water, stirring for 0.5 hour, centrifuging for 30 minutes at speed of 7000 rpm, removing supernatant, repeating to supernatant pH value of 7, adding precipitated solid to 20 mL deionized water, ultrasonically treating for 1 hour, centrifuging for 45 minutes at speed of 7000 rpm, and vacuum drying solid at 70 degrees C for 24 hours to obtain graphene oxide (GO); (D) adding 5-5.5 g GO into 200 mL beaker, adding 25-30 mL sulfone and 25-30 mL absolute ethanol, stirring at room temperature for 6 hours, and filtering solid left on filter paper with 10-15 mL anhydrous alcohol to obtain filtrate; (E) transferring into 250 mL flask filled with nitrogen, adding 25-40 mL absolute ethanol, ultrasonically treating for 20 minutes, adding 15-20 mL allyl acetoacetate and 2-3 mL acrylic acid, putting flask into constant temperature water bath at 65 degrees C, continuously stirring for 20 minutes, adding 1.5-2 g azobisisobutyronitrile as initiator, continuously stirring for 12 hours, reacting for 12 hours, filtering solution, washing with 20 mL anhydrous ethanol to remove impurity, and vacuum drying solid to 70 degrees C for 24 hours to obtain allyl acetoacetate functionalized graphene oxide (GO-A); and (F) adding wastewater containing cadmium ion into beaker, adjusting pH value to 7, adding GO-A, constant velocity stirring for 2 hours, filtering, obtaining GO-A, dispersing with 0.01 mol/L nitric acid, adjusting to pH value to 1, ultrasonically oscillating for 5 minutes, filtering, rinsing with 50 mL anhydrous ethanol, and vacuum drying solid to 70 degrees C for 24 hours.