• 专利标题:   Graphene-based sulfonic acid catalyst for catalyzing alkylation reaction of cresol, is prepared by bonding benzene ring to graphene through covalent grafting, and grafting sulfonate groups on edge of graphene.
  • 专利号:   CN113244955-A, CN113244955-B
  • 发明人:   FENG Y, CHENG J, WANG Z, FAN S, XIE D, WANG S
  • 专利权人:   UNIV HEFEI TECHNOLOGY
  • 国际专利分类:   B01J031/02, C07C001/32, C07C015/04, C07C303/06, C07C309/29, C07C037/14, C07C039/06
  • 专利详细信息:   CN113244955-A 13 Aug 2021 B01J-031/02 202180 Pages: 14 Chinese
  • 申请详细信息:   CN113244955-A CN10563550 24 May 2021
  • 优先权号:   CN10563550

▎ 摘  要

NOVELTY - A graphene-based sulfonic acid catalyst is prepared by bonding benzene ring to graphene through covalent grafting, and grafting sulfonate groups on the edge of graphene or covalently modified benzene ring through sulfonation reaction. USE - Graphene-based sulfonic acid catalyst for catalyzing alkylation reaction of cresol (claimed). ADVANTAGE - The graphene-based sulfonic acid catalyst has high-efficiency activity for aromatic alkylation reactions, and exhibits similar catalytic efficiency to concentrated sulfuric acid. DETAILED DESCRIPTION - A graphene-based sulfonic acid catalyst is prepared by bonding benzene ring to graphene through covalent grafting, and grafting sulfonate groups on the edge of graphene or covalently modified benzene ring through sulfonation reaction. The graphene-based sulfonic acid catalyst comprises graphene-containing compound of formula (I). INDEPENDENT CLAIMS are included for the following: (1) preparation of the graphene-based sulfonic acid catalyst, which involves (1) adding graphene, aniline, concentrated sulfuric acid and deionized water into flask, stirring to make reaction liquid, placing the flask in an ice water bath to cool to 0 degrees C, adding sodium nitrite in drops to the reaction solution for 1.0-1.5 hours, reacting at room temperature for 2-24 hours, cooling the reaction mixture to room temperature, performing suction filtration, obtaining solid, washing with deionized water, ethanol and acetone successively, obtaining graphene-based material after vacuum drying, (2) adding graphene-based material to flask, adding sulfonation reagent under stirring conditions at 80-200 degrees C for sulfonation reaction, cooling the reaction mixture to room temperature, washing the product with deionized water and acetone, washing until the filtrate is neutral, using barium hydroxide to determine the end of the washing, and vacuum drying; (2) use of the graphene-based sulfonic acid catalyst to catalyze alkylation reaction of cresol; and (3) alkylation reaction of cresol using the graphene-based sulfonic acid catalyst, which involves adding cresol and graphene-based sulfonic acid catalyst to reactor, turning on the stirring, controlling the reaction mixture to an appropriate temperature, passing isobutylene gas into the reaction mixture at a determined flow rate, sampling at regular intervals, detecting the content of cresol in the reaction mixture by gas chromatography, monitoring the progress of the reaction until the reaction of the raw material m-cresol is complete, filtering the reaction mixture while it is hot, separating and recovering the graphene-based sulfonic acid catalyst, separating the reaction solution and purifying by vacuum distillation to separate and purify the unreacted raw material cresol and the mono-alkylation and double-alkylation products of the cresol.