Patent GB-1379847-A (GB)
Title: Method of preparing a hydrorefining catalyst
IPC: B01J23/652
Filed: 1972-03-24
Abstract: 1379847 Hydrocarbon hydrorefining catalysts UNIVERSAL OIL PRODUCTS CO 24 March 1972 [25 March 1971] 13819/72 Heading B1E [Also in Division C5]  Hydrocarbon hydrorefining catalyst comprising a Group VIB metal component and a Group VIII metal component is prepared by a method wherein refractory inorganic oxide carrier material is impregnated with an aqueous solution containing a soluble compound of a Group VIB metal and a soluble compound of a Group VIII metal and, after evaporating water therefrom, is calcined initially at a temperature of from 100 to 427‹C (212 to 800‹F) for a period of at least ¢ hour (for example at a temperature of from 260 to 427‹C (500 to 800‹F) for a period of from ¢ to 2 hours in an atmosphere containing less than 50 volume per cent steam, preferably substantially dry air) and thereafter at a temperature of from 427 to 621‹C (800 to 1150‹F) for a period of from 1 to 4 hours in an atmosphere containing at least 25, preferably from 60 to 80, volume per cent steam, the volume ratio of impregnating solution to carrier material being from 0.5:1 to 2:1, preferably from 0.6:1 to 1:1, for example about 0.7:1. Evaporation of water, which preferably is such as to provide material which exhibits a loss on ignition at 500‹C of less than 50, preferably from 35 to 45, weight per cent, may be effected for a period not greater than 4 hours. The refractory inorganic oxide carrier material may be alumina, silica, zirconia, boria, thoria or a combination thereof, for example silica-alumina having an Al 2 O 3 :SiO 2  molar ratio of at least 1:1, preferably an Al 2 O 3 :SiO 2  weight ratio of from 3:1 to 9:1; the carrier material preferably has a surface area of from 175 to 380m<SP>2</SP>/g, an average pore volume of from 0.5 to 0.9 ml/g and an average pore diameter of from 70 to 200 Angstroms. The metal of the Group VIB metal component may be selected from chromium, molybdenum and tungsten; the metal of the Group VIII metal component may be selected from iron, cobalt, nickel, ruthenium, rhodium. palladium, osmium, iridium and platinum; the Specification gives examples of suitable Group VIB metal compounds and Group VIII metal compounds for use in the preparation of the catalyst which may contain from 5 to 20 weight per cent molybdenum and from 0.1 to 10 weight per cent nickel. As exemplified, 1.6 mm spheres of silica-alumina containing 88 weight per cent Al 2 O 3  and 12 weight per cent SiO 2  and having a surface area of 285 m<SP>2</SP>/g, an average pore volume of 0.7 ml/g and an average bulk density of 0.44 g/ml are impregnated with a solution prepared by dissolving molybdic acid and nickel nitrate in aqueous ammonia and, after evaporating water therefrom over a period of 4 hours, are calcined initially at 343‹C (650‹F) for 1 hour in dry air and thereafter at 552‹C (1025‹F) for 2 hours in air containing 70 volume per cent steam to provide material haying a surface area of 150 m<SP>2</SP>/g, an average pore volume of 0.45 ml/g and an average pore diameter of 115 Angstroms, which material is used in the form of a plurality of beds separated by sand in a process for hydrorefining a residual crude oil.