Mesocarbon microbeads of narrow particle-size distribution are produced by: subjecting a heavy oil to a primary heat treatment at a temperature T1 to prepare a pitch containing mesophase microspheres; once cooling this pitch to a temperature lower than its softening point; thereafter subjecting the pitch to a secondary heat treatment at a temperature T2, which is higher than 350 DEG C. and lower than (T1-40 DEG C.); cooling the pitch at a cool rate lower than 200 DEG C./hour; separating from the pitch mesophase microspheres which precipitated in the secondary heat-treatment step; and thereafter obtaining by solvent extraction mesophase microspheres of substantially uniform particle size formed in the residual pitch. The mesocarbon beads of narrow particle-size distribution thus obtained are particularly suitable for use as chromatograph packing material, catalyst support, and other uses.
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