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 additional 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 electrosynthesis 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.