A process is developed for the autoclave leaching of nickel and manganese with sulfuric acid from the products of catalytic synthesis of industrial diamonds containing 20% Ni and 30% Mn. The optimum conditions for the autoclave processes are determined to be as follows: the temperature range is 150–160°C, the solution acidity is 5 N H₂SO₄ (230–240 g/l), the leaching duration is 2 h, and the number of processing steps is two. The extraction of the metals into a solution under these conditions is >99% for a total Ni + Co content of <0.4–0.5% in the autoclave leaching cake. The studies performed are related to the search for alternative ways of the catalytic preparation of industrial diamonds that can replace the nonferrous metal leaching technology using aqua regia solutions, which is mainly applied for these purposes under industrial conditions.