▎ 摘 要
NOVELTY - Preparation of electrode involves dispersing (i) a carbon material and a copper-based macrocyclic compound in a solvent, ultrasonically-stirring, removing the solvent by rotary evaporation, drying, heat-treating in a mixed atmosphere of hydrogen, helium, nitrogen, argon and/or ammonia to obtain a copper-based macrocyclic compound/carbon electrocatalyst, immersing (ii) a copper base material in a mixed solvent of ethanol, isopropanol, acetone and/or dilute hydrochloric acid, rinsing with deionized water, vacuum-drying and cutting to obtain a copper substrate, adding (iii) the copper-based macrocyclic compound/carbon electrocatalyst, water, alcohol and Nafion (RTM: sulfonated tetrafluoroethylene-based fluoropolymer-copolymer) in sequence, ultrasonically-dispersing to obtain a catalyst slurry, and coating the catalyst slurry on the copper substrate to obtain a copper electrode loaded with electrocatalyst, and heating (iv) the copper electrode loaded with electrocatalyst. USE - Preparation of electrode used in electrocatalytic reduction reaction of carbon dioxide (all claimed). ADVANTAGE - The method enables simple, easy, environmentally-friendly and large-scale preparation of electrode under mild reaction conditions. The stability and conductivity of the catalyst are improved by controlling the conditions of heat treatment temperature, atmosphere and duration. The electrode enables electrocatalytic reduction reaction of carbon dioxide with high product selectivity at low potential. DETAILED DESCRIPTION - Preparation of electrode involves dispersing (i) a carbon material and a copper-based macrocyclic compound in a solvent, ultrasonically-stirring at 20-60 degrees C for 3-10 hours, removing the solvent by rotary evaporation, drying, heat-treating at 200-900 degrees C for 1-5 hours in a mixed atmosphere of hydrogen, helium, nitrogen, argon and/or ammonia to obtain a copper-based macrocyclic compound/carbon electrocatalyst, immersing (ii) a copper base material in a mixed solvent of ethanol, isopropanol, acetone and/or dilute hydrochloric acid at 20-60 degrees C for 10-40 minutes, rinsing with deionized water, vacuum-drying and cutting to obtain a copper substrate, adding (iii) the copper-based macrocyclic compound/carbon electrocatalyst, water, alcohol and Nafion (RTM: sulfonated tetrafluoroethylene-based fluoropolymer-copolymer) in sequence, ultrasonically-dispersing for 0.1-1 hour to obtain a catalyst slurry, and coating the catalyst slurry on the copper substrate to obtain a copper electrode loaded with electrocatalyst, and heating (iv) the copper electrode loaded with electrocatalyst in a mixed atmosphere of hydrogen, helium, nitrogen, argon and/or ammonia at 500-1000 degrees C for 1-5 hours.