Practical CO2 adsorption processes require adsorbents that can be easily and quickly synthesized at a reasonable cost, while maintaining a significant adsorption performance. In this research, a metal organic framework based on Cu and H3BTC was synthesized by the potentiodynamic method. Results showed that the nature of the solvent strongly affected the phase structure, morphology and specific surface area of the obtained material. In methanol, a mixture of 1D structure Cu‐BTC (catena‐triaqua μ‐[1,3,5‐benzenetricarboxylato]‐copper (II) corresponding to the formula [Cu(BTC)(H2O)3)]n and micropillars structure Cu(BTC).3H2O was obtained. The 1D structure Cu‐BTC had a plate shape and a small specific surface area of 21 m2/g. In ethanol, the 3D structure Cu‐BTC (Cu3(BTC)2) was successfully synthesized. The obtained material has a cubic shape of size from 50 nm to 500 nm and a much better specific surface area of 620 m2/g. The 3D structure Cu‐BTC offered a high CO2 adsorption capacity of 3.6 mmol/g at standard conditions, and 1.6 mmol/g at more realistic conditions.