A method for preparing Group VIII metal-phosphorus compounds supported on a high surface area solid support selected from the group consisting of carbon, alumina, silica, silica-alumina, zeolite, kieselguhr, vermiculite, the refractory oxides of Group IVb and Vb transition metals and mixtures thereof, wherein the Group VIII metal-phosphorus crystallite size is about 300 A or less, wherein the process consists of the steps of:
- (a) impregnating said high surface area support with a solution of at least one water soluble Group VIII metal salt selected from the group consisting of water soluble Group VIII metal chloride, Group VIII metal nitrate and Group VIII metal ammonia complexes;
- (b) impregnating said support with phosphorus by means of a phosphorus source selected from the group consisting of elemental phosphorus and at least one water soluble phosphate salt, in an amount sufficient to resalt in a phosphorus to Group VIII metal atomic ratio of about 0.3 to about 3.0;
- (c) reducing the reducible deposited components resultant from the completion of steps (a) and (b) in a gaseous reducing atmosphere at a temperature in the range of about 200.degree. C. to about 650.degree. C. for a time sufficient to generate the desired supported Group VIII metal-phosphorus compounds.