• 专利标题:   Modifying coconut shell activated carbon with oxidized graphene is useful for chlorination comprises preparing graphene oxide; dispersing in solvent, adding cationic polymer into dispersion of graphene oxide and magnetically agitating.
  • 专利号:   CN107500292-A, CN107500292-B
  • 发明人:   MIAO J, WANG J, HUANG Y, WANG C, BAO L
  • 专利权人:   JIANGSU SULI FINE CHEM CO LTD
  • 国际专利分类:   C01B032/354
  • 专利详细信息:   CN107500292-A 22 Dec 2017 C01B-032/354 201808 Pages: 8 Chinese
  • 申请详细信息:   CN107500292-A CN10873762 25 Sep 2017
  • 优先权号:   CN10873762

▎ 摘  要

NOVELTY - Modifying coconut shell activated carbon with oxidized graphene comprises preparing graphene oxide; dispersing in solvent to prepare graphene oxide, then adding cationic polymer into the dispersion of graphene oxide, magnetically agitating to obtain grapheme oxide/cationic polymer colloidal solution composition; the solvent is distilled water, ethanol, methanol, toluene, dimethylformamide and/or carbon tetrachloride; taking activating agent in impregnating pool, the activator is potassium hydroxide, sodium hydroxide and/or potassium carbonate, and adding distilled water. USE - The modifying coconut shell activated carbon with oxidized graphene is useful for chlorination (claimed). ADVANTAGE - The method greatly reduces the temperature required for the chlorination reaction and increases the product content ( greater than or equal to 99.6%), reduces the volume of catalyst to 50%; the conversion rate of raw material is greater than or equal to 96.3%, the production of chlorinated products content is greater than or equal to 99.6% and the coconut shell activated carbon has shelf life of 1400-1450 hours, greatly improves the utilization of the catalyst, reduces production costs and is economical. DETAILED DESCRIPTION - Modifying coconut shell activated carbon with oxidized graphene comprises (i) preparing graphene oxide; (ii) dispersing the step (i) in the solvent to prepare the graphene oxide, then adding cationic polymer into the dispersion of graphene oxide, magnetically agitating for 2-4 hours at room temperature to obtain grapheme oxide/cationic polymer colloidal solution composition, the cationic polymer is 3-5 wt.% of graphene oxide; the solvent is distilled water, ethanol, methanol, toluene, dimethylformamide (DMF) and/or carbon tetrachloride; (iii) taking 2.4-4.8 g activating agent in the impregnating pool, the activator is potassium hydroxide (KOH), sodium hydroxide (NaOH) and/or potassium carbonate (K2CO3), then adding 800-1000 l distilled water into the dipping pool, stirring and dissolving the activating agent completely to form solution, taking 300-600 g coconut shell active carbon in the activator solution for 12-16 hours to finish activation of coconut shell active carbon, (iv) mixing graphene oxide/cationic polymer complex solution prepared in step (ii) into step (iii) by activation of coconut shell active carbon, stirring slowly for 2-4 hours, filtering the coconut shell active carbon, drying to obtain the graphene oxide/coconut shell active carbon material composition, graphene oxide is coconut shell active carbon, 3-5 wt.% graphene oxide in the preparation process on the surface with coconut shell of positively charged cationic polymer and the negatively charged activated carbon electrostatic self-assembly function to prepare the material composition; (v) modifying the activated coconut shell active carbon in the step (iv) to prepare the graphene oxide modified coconut shell active carbon is filled into the composite bed reactor, the composite bed reactor is fluidized bed and fixed bed composite bed reactor; the compound bed reactor into the excessive chlorine, activated and modified active carbon at 90-120 degrees C, and activation for 1-3 hours, where two reactors each point temperature is stable, not detected in tail gas hydrogen chloride gas, as the activation (vi) placing the raw material into the melting by a metering feeder, then placing raw material into the vaporizer, and introducing preheated nitrogen together with the vaporizer, for vaporizing the raw material; the raw material is benzonitrile, 2-cyano-pyridine; (vii) adding liquid chlorine into chlorine after vaporizing and preheating, then raw material gas contains nitrogen 70 wt.% chlorine and mixing with step (vi), introducing the step (iii) into the fluidized bed, finishing the first step reaction of gas in the fluidized bed and then into fixed bed in the supplementary reaction is carried out by mixing with the remaining 30 wt.% chlorine, (viii) collecting the reactant to obtain the sodium chloride product powder, the chlorinated product is 5-chloro-benzonitrile, 2-cyano-pyridine or tetrachloro-m-(p)-benzene.