Acid activation of clay minerals is one of the most effective methods for production of materials with increased acidity and porosity. In this review, the benefits of infrared (IR) spectroscopy in studies of acid-treated clay minerals are demonstrated. Protons penetrating into the clay mineral layers evoke structural modifications that can be followed readily by changes in the characteristic absorption bands attributed to the vibrations of the OH and Si–O groups. In the first part of the review the effect of the clay mineral type, composition, layer charge, non-swelling layers, and organo-modification on the dissolution rate is reported. The identification of the acid sites via pyridine adsorption also included. The purpose was to gather the IR results published in previous studies in a single summary paper. In the second part select recent studies reporting the utilization of IR spectroscopy for the characterization of acid-activated clay minerals, mainly applied as catalysts or adsorbents, are discussed. IR spectroscopy as a simple and non-destructive technique deserves attention also today.