A microwave reactor (Synthos 3000) was used to synthesize a microporous copper metal-organic framework (Cu-MOF), Cu(hfipbb)(H2hfipbb)0.5 [H2hfipbb = 4,4′-(hexafluoroisopropylidene) bis(benzoic acid)] aiming at reducing the synthesis time, increasing the MOF yield and improving the MOF quality. The scanning electron microscopy (SEM) images of the MOF samples obtained in this work reveal that the microwave-synthesized Cu-MOF samples have a more uniform particle size distribution and a smaller particle size. The pore textural properties obtained by adsorption of carbon dioxide at 0°C indicate that the microwave-synthesized Cu-MOF samples have a similar pore structure as that of the MOF synthesized by the conventional hydrothermal method. The cubic structure of this Cu-MOF is also confirmed by X-ray powder diffraction results. Adsorption equilibrium and kinetics of CO2 and CH4 on the microwave-synthesized Cu-MOF adsorbents were also determined at various temperatures and gas pressures up to 1 bar. The combined equilibrium and kinetic selectivity was calculated from the adsorption isotherms and the adsorption kinetic plots. Separation a CO2/CH4 mixture by the Cu-MOF adsorbent was demonstrated in a gas chromatograph column packed with the Cu-MOF adsorbent.