• 专利标题:   Preparation of sulfonic acid-sulfide mixed hybrid graphene catalyst for preparing 5-hydroxymethylfurfural carbohydrate, involves mixing mixed sulfide graphene and concentrated sulfuric acid, reacting mixture and drying product.
  • 专利号:   CN104971772-A, CN104971772-B
  • 发明人:   LI S, LI Z, SU K, SONG H
  • 专利权人:   UNIV TIANJIN POLYTECHNIC
  • 国际专利分类:   B01J031/02, C07D307/46
  • 专利详细信息:   CN104971772-A 14 Oct 2015 B01J-031/02 201625 Pages: 7 Chinese
  • 申请详细信息:   CN104971772-A CN10308998 08 Jun 2015
  • 优先权号:   CN10308998

▎ 摘  要

NOVELTY - Sulfonic acid-sulfide mixed hybrid graphene catalyst is prepared by uniformly mixing 0.05-1 g mixed sulfide graphene and 10-30 mL 98% concentrated sulfuric acid, stirring at 40-80 degrees C, adding 0.12-0.24 g fuming sulfuric acid or chlorosulfonic acid, reacting for 1-3 hours, adding excess of deionized water to reaction mixture to form precipitate, washing precipitate with deionized water to neutral and drying washed product. USE - Preparation of sulfonic acid-sulfide mixed hybrid graphene catalyst used for preparing 5-hydroxymethylfurfural carbohydrate (claimed). ADVANTAGE - The method enables preparation of sulfonic acid-sulfide mixed hybrid graphene catalyst having excellent catalytic activity, agglomeration resistance and selectivity by simple, efficient and environmentally-friendly method. The 5-hydroxymethylfurfural carbohydrate is prepared with high carbohydrate conversion rate and yield under mild reaction conditions, using sulfonic acid-sulfide mixed hybrid graphene catalyst. DETAILED DESCRIPTION - Mixed sulfide graphene is prepared by stirring 0.1-1 g graphene and 5-20 ml alkyl halide (a) at 20-50 degrees C, adding 0.2-3 g halogen, reacting mixture at 10-80 degrees C, distilling off unreacted halide (a) and halogen, adding 10-50 ml organic amine solvent, stirring, adding 0.1-1 g anhydrous sulfide, reacting at 130-170 degrees C for 2-6 hours, adding 0.3-1 g halide (b), reacting at 140-180 degrees C for 2-6 hours, stopping reaction, cleaning product, removing reaction residue and drying product. Sulfonic acid-sulfide mixed hybrid graphene catalyst is prepared by uniformly mixing 0.05-1 g mixed sulfide graphene and 10-30 mL 98% concentrated sulfuric acid, stirring at 40-80 degrees C, adding 0.12-0.24 g fuming sulfuric acid or chlorosulfonic acid, reacting for 1-3 hours, adding excess of deionized water to reaction mixture to form precipitate, washing precipitate with deionized water to neutral and drying washed product. An INDEPENDENT CLAIM is included for sulfonic acid-sulfide mixed hybrid graphene catalyst for preparation of 5-hydroxymethylfurfural carbohydrate, which involves adding 70-110 mg catalyst to 3-7 ml ionic liquid, adding 0.6-1.2 g carbohydrate, reacting mixture at 130-180 degrees C for 1-8 hours and extracting with ethyl acetate.