Dolomite as a heterogeneous catalyst can be used in biodiesel synthesis. Process material costs can be reduced by regenerating and reusing the catalyst. Two methods of regeneration of dolomite were studied: (1) washing for 30 min with methanol, filtration, and washing for 30 min with hexane and (2) calcination at high temperature. Catalytic efficiency and catalyst changes after 1–6 cycles were evaluated. X-ray, FTIR, and SEM studies were performed. Calcination has been found to be a more effective method of catalyst regeneration than washing with solvents. The catalytic effectiveness of dolomite only slightly decreased over six application cycles. The results of the instrumental analysis showed that the structure and composition of the dolomite do not change during calcination after three cycles, while obvious changes in the structure of dolomite during catalyst washing were observed.