Metal-organic frameworks (MOFs)-derived materials with a large specific surface area and rich pore structures are favorable for catalytic performance. In this work, MOFs are successfully prepared. Through pyrolysis of MOFs under nitrogen gas, zinc-based catalysts with different active sites for acetylene acetoxylation are obtained. The influence of the oxygen atom, nitrogen atom, and coexistence of oxygen and nitrogen atoms on the structure and catalytic performance of MOFs-derived catalysts was investigated. According to the results, the catalysts with different catalytic activity are Zn-O-C (33%), Zn-O/N-C (27%), and Zn-N-C (12%). From the measurements of X-ray photoelectron spectroscopy (XPS), it can be confirmed that the formation of different active sites affects the electron cloud density of zinc. The electron cloud density of zinc affects the ability to attract CH3COOH, which makes catalysts different in terms of catalytic activity.