Electrosynthesis of HKUST-1 with flow-reactor post-processing

Abstract

Electrochemical synthesis has been proposed as an efficient method for cost-effective and large-scale production of metal-organic frameworks (MOFs). This work investigates the combined electrochemical synthesis with flow synthesis post-treatment for the production of high surface area HKUST-1. The electrochemical synthesis process used in the experimental work did not require addi-tional electrolytes or washing of the synthesis product. Batch electrosynthesis and electrosynthesis with flow synthesis were compared for the quality of the product using Brunauer–Emmett–Teller (BET) surface area, X-ray diffraction (XRD), and scanning electron microscopy (EIS). Batch elec-trosynthesis in 0.01 M benzene-1,3,5-tricarboxylic acid (H3BTC) solution produced HKUST-1 with BET surface area of 1550 m2/g which was increased further to 1716 m2/g with post-flow-synthesis treatment. The greatest change in surface area after flow processing was observed when using 0.78 M H3BTC, with corresponding surface areas of 481 m2/g and 1531 m2/g. According to SEM and BET results, the product purity improved during the post-flow-synthesis treatment. The proposed method enables continuous flow synthesis of high-quality MOFs with minimal purification steps.