• 专利标题:   Synthesis of symmetrical disulfide by dissolving insoluble copper salt and amine in methanol to form mixed solution, dispersing graphene in methanol to form dispersion liquid, mixing halide, elemental sulfur, copper-based catalyst, acid binding agent and solvent and carry out post-processing.
  • 专利号:   CN114989050-A
  • 发明人:   CHEN X, ZHOU S, RUAN J, JIN H, QIAN C
  • 专利权人:   UNIV ZHEJIANG, UNIV ZHEJIANG QUZHOU RES INST
  • 国际专利分类:   B01J031/02, C07C319/24, C07C321/14, C07C321/20, C07C321/28, C07D213/61
  • 专利详细信息:   CN114989050-A 02 Sep 2022 C07C-319/24 202292 Chinese
  • 申请详细信息:   CN114989050-A CN10778833 30 Jun 2022
  • 优先权号:   CN10778833

▎ 摘  要

NOVELTY - Synthesis method of symmetrical disulfide compound involves (S1) dispersing and dissolving insoluble copper salt and amine auxiliary agent in methanol to obtain a mixed solution, dispersing graphene in methanol to obtain a dispersion liquid, mixing the mixed solution with the dispersion liquid, leaving the obtained precipitate for drying and calcining in an inert gas containing 5±1% of ammonia gas to obtain a copper-based loaded type catalyst. The mol ratio of the insoluble copper salt to amine auxiliary agent is 1:(1-2), and (S2) mixing halide, elemental sulfur, copper-based supported catalyst, acid binding agent and solvent obtained in step (S1), and stirring to react, the molar ratio of the halide, elemental sulfur and acid-binding agent is 1:(1.5-2.5):2, the copper-based supported catalyst is 5-10% of the mass of the halide, after the reaction is completed and carrying out post-processing to obtain the symmetric disulfide compound. USE - The method is used for synthesizing symmetrical disulfide compound. ADVANTAGE - The method is simple and environmentally-friendly, has high yield, and excellent selectivity. DETAILED DESCRIPTION - Synthesis method of symmetrical disulfide compound involves (S1) dispersing and dissolving insoluble copper salt and amine auxiliary agent in methanol to obtain a mixed solution, dispersing graphene in methanol to obtain a dispersion liquid, mixing the mixed solution with the dispersion liquid, leaving the obtained precipitate for drying and calcining is carried out at 400-600℃ for 5±0.5 hours in an inert gas containing 5±1% of ammonia gas to obtain a copper-based loaded type catalyst. The mol ratio of the insoluble copper salt to amine auxiliary agent is 1:(1-2) and the mass ratio of the copper salt to graphene is 1:(50-100), and (S2) mixing halide, elemental sulfur, copper-based supported catalyst, acid binding agent and solvent obtained in step (S1), and stirring to react at 60-100℃ for 6-10 hours, the molar ratio of the halide, elemental sulfur and acid-binding agent is 1:(1.5-2.5):2, the copper-based supported catalyst is 5-10% of the mass of the halide, after the reaction is completed and carrying out post-processing to obtain the symmetric disulfide compound.