A highly functional, environmentally friendly carbonaceous adsorbent material using black liquor (a by-product from the pulp manufacturing) was produced and characterized. This study showed the effect of self-chemical activation driven by inherent alkali, originated from the unique composition of black liquor. A preparation of the micropore-dominant activated carbon was made in an easy and simple manner. The specific surface areas of samples were found to be 718–1591 m2/ g variated upon heat treatment conditions. The sample activated at 850 °C (50 min as retention time) showed the maximum specific surface area of 1591 m2/ g with 13.6% as a production yield. Considering the factors influencing pore structure of activated carbon materials in this study, it was confirmed that mesopore-related surface area increased gradually as the activation temperature and retention time increased. It is noteworthy to address that economically valuable micropore-dominant activated carbon can be produced by a simple heat treatment of the waste material, black liquor. The activated carbon sample derived from black liquor can be applied to various fields, such as environment and energy storage.