This invention provides a process for preparing carboxylic acid, the process comprising subjecting an oxidation product produced by reacting a peroxide with (a) unsaturated aliphatic monocarboxylic acid having at least one unsaturated bond in the carbon chain and containing 6 to 24 carbon atoms or its ester or (b) cyclic and/or acyclic aliphatic olefin having at least one unsaturated bond in the carbon chain to oxidation by oxygen or oxygen-containing gas in the presence of a catalyst comprising (i) at least one heavy metal compound and (ii) at least one member selected from the group consisting of a bromine compound and a chlorine compound.