• 专利标题:   Green synthesis of mercaptan compound by dissolving soluble nickel salt and amine auxiliary agent in ethanol, dispersing graphene in ethanol, mixing, calcining in inert gas, mixing chloride, sulfur, acid binding agent and solvent, carrying out magnetic stirring reaction and post-processing.
  • 专利号:   CN115010632-A
  • 发明人:   CHEN X, ZHOU S, RUAN J, LI Y, QIAN C
  • 专利权人:   UNIV ZHEJIANG, UNIV ZHEJIANG QUZHOU RES INST
  • 国际专利分类:   B01J021/18, B01J023/755, B01J027/24, B01J037/02, C07C319/02, C07C321/04, C07C321/26
  • 专利详细信息:   CN115010632-A 06 Sep 2022 C07C-319/02 202297 Chinese
  • 申请详细信息:   CN115010632-A CN10801094 07 Jul 2022
  • 优先权号:   CN10801094

▎ 摘  要

NOVELTY - A green synthesis method of mercaptan compound comprises (S1) dissolving soluble nickel salt and an amine auxiliary agent in ethanol to obtain a mixed solution, dispersing graphene in ethanol to obtain a dispersion liquid, mixing the mixed solution with the dispersion liquid, leaving to obtain a precipitate, drying and calcining the precipitate in inert gas containing 5 ± 1% ammonia gas at 400-600℃ for 5 ± 0.5 hours to obtain a nickel-based supported catalyst; where the molar ratio of the nickel salt and the amine auxiliary agent is 1:1-2, and the mass ratio of the nickel salt and the graphene is 1:40-100, and (S2) mixing chloride, elemental sulfur, the nickel-based supported catalyst obtained in step (S1), an acid binding agent and a solvent, carrying out magnetic stirring reaction at 60-110℃ for 12-24 hours and after completing the reaction, post-processing to obtain the product. USE - The green method is used for the synthesis of mercaptan compound. ADVANTAGE - The invention catalyzes the C-S coupling reaction of chloride and elemental sulfur to directly generate mercaptan compound. The yield of mercaptan compound reaches 83-96%. DETAILED DESCRIPTION - A green synthesis method of mercaptan compound comprises (S1) dissolving soluble nickel salt and an amine auxiliary agent in ethanol to obtain a mixed solution, dispersing graphene in ethanol to obtain a dispersion liquid, mixing the mixed solution with the dispersion liquid, leaving to obtain a precipitate, drying and calcining the precipitate in inert gas containing 5 ± 1% ammonia gas at 400-600℃ for 5 ± 0.5 hours to obtain a nickel-based supported catalyst; where the molar ratio of the nickel salt and the amine auxiliary agent is 1:1-2, and the mass ratio of the nickel salt and the graphene is 1:40-100, and (S2) mixing chloride, elemental sulfur, the nickel-based supported catalyst obtained in step (S1), an acid binding agent and a solvent, carrying out magnetic stirring reaction at 60-110℃ for 12-24 hours and after completing the reaction, post-processing to obtain the product; where the molar ratio of the chloride, elemental sulfur and the acid binding agent is 1:1.5:2, and the mass of the nickel-based supported catalyst is 3.5-10% of that of the chloride.