• 专利标题:   Preparing 2,5-dimethylfuran by catalytically hydrogenating 5-hydroxymethylfurfural comprises taking ethanol as solvent, reacting 5-hydroxymethylfurfural with hydrogen under action of nickel-iron/reduced graphene oxide catalyst.
  • 专利号:   CN112778243-A, CN112778243-B
  • 发明人:   ZHOU J, LV Y, MAO J, LI S, YIN J
  • 专利权人:   UNIV DALIAN
  • 国际专利分类:   B01J023/755, B01J037/00, B01J037/02, B01J037/08, B01J037/12, B01J037/16, C07D307/36
  • 专利详细信息:   CN112778243-A 11 May 2021 C07D-307/36 202148 Pages: 8 Chinese
  • 申请详细信息:   CN112778243-A CN10007179 05 Jan 2021
  • 优先权号:   CN10007179

▎ 摘  要

NOVELTY - Preparing 2,5-dimethylfuran by catalytically hydrogenating 5-hydroxymethylfurfural comprises taking ethanol as solvent, and reacting 5-15 wt.% 5-hydroxymethylfurfural with hydrogen under the action of nickel-iron/reduced graphene oxide catalyst at 180-220 degrees C for 1-3 hours with hydrogen pressure of 1-4 MPa. USE - The method is useful for preparing 2,5-dimethylfuran by catalytically hydrogenating 5-hydroxymethylfurfural. ADVANTAGE - The method has 100% conversion rate of 5-hydroxymethylfurfural, provides 97% 2,5-dimethylfuran yield. DETAILED DESCRIPTION - An INDEPENDENT CLAIM is also included for catalyst for preparing 2,5-dimethylfuran, comprising (i) taking 230 ml concentrated sulfuric acid and 5 g sodium nitrate, stirring, adding 10 g natural crystalline flake graphite powder, stirring for 2.5 hours, adding 30 g potassium permanganate, transferring into constant temperature water bath and reacting at 35 degrees C for 2 hours, adding 460 ml deionized water, stirring in oil bath at 98 degrees C for 15 minutes, adding 1.4 l deionized water for stopping the reaction, adding 25 ml hydrogen peroxide (30%), cooling at room temperature, adding deionized water, centrifuging and washing until neutrality to obtain past-like graphene oxide GO, measuring dry basis content to 1 wt.%, taking past-like graphene oxide GO, dispersing in 1000 ml deionized water, ultrasonically processing for 30 minutes, allowing to stand, aging, adding 25 ml aqueous ammonia (30%) and 6 ml hydrazine hydrate (80%), refluxing in oil bath at 95 degrees C for 3 hours, adding 4 ml hydrazine hydrate (80%), reacting for 30 minutes, adding 4% hydrochloric acid solution, filtering during hot, freezing and drying to obtain reduced graphene oxide carrier; (ii) dissolving nickel nitrate hexahydrate and iron (III) nitrate nonahydrate in 0.85 ml deionized water to obtain a salt solution; (iii) adding salt solution into a beaker, adding 0.2 ml absolute ethanol and 100 mg reduced graphene oxide carrier, continuously stirring with glass rod, and placing the sample at room temperature for 3 hours; (iv) placing the sample in a vacuum drying oven at 50 degrees C for 12 hours, and grinding the sample into a powdered sample with an agate mortar; (v) adding powdered sample obtained in step (iv) into a quartz tube and placing in a tube furnace under nitrogen atmosphere, heating from room temperature to 500 degrees C with a heating rate of 10 degrees C/minute, baking at a constant temperature of 500 degrees C for 2 hours, cooling, taking out the sample and storing in a sealed container.