Using an environmentally friendly method to produce a stable and highly catalytically active electrocatalyst for the oxygen evolution reaction (OER) is becoming increasingly urgent. Herein, a novel bimetallic metal-organic framework (MOF), specifically a copper-cobalt 1, 3, 5-benzenetricarboxylate (Cu-Co-BTC) MOF, was successfully prepared by employing the gas-solid two-phase flow (GSF) synthetic technique. The as-prepared Cu-Co-BTC with its multiple active sites afforded a current density of 10 mA cm-2 at 239 mV for the OER in a 1 mol L-1 KOH solution, and showed a better electrocatalytic performance than did single-metal-containing Cu-BTC and Co-BTC materials. This work provides a new idea, one involving using novel gas-solid phase reactions for the preparation of electrocatalysts in large quantities.