Method of preparing a catalyst for use in the hydrotreating of high boiling hydrocarbon feedstocks

A process for hydrotreating a change hydrocarbon feed containing components boiling above 1000° F., and sediment-formers, sulfur, metals, asphaltenes, carbon residue, and nitrogen which comprises

• passing said charge hydrocarbon feed and hydrogen through a reactor under isothermal hydrotreating conditions in the presence of a catalyst comprising a porous alumina support having incorporated therein about 1.1 to 6 wt. % of a Group VIII metal oxide, and about 5 to 24 wt. % of a Group VI-B metal oxide, to provide a liquid and gaseous effluent containing a hydrotreated product, and
• recovering said hydrotreated product containing a decreased content of components boiling above 1000° F., sediment, sulfur, metals, carbon residue, asphaltenes and nitrogen,
• said catalyst having been prepared by mulling a porous alumina powder with a salt of a Group VIII metal oxide and with a salt of a Group VI-B metal oxide in the presence of an acid to provide a mixture, extruding the mixture to form an extrudate, drying the extrudate and subjecting the dried extrudate to hydrothermal calcination to provide said catalyst,
• said catalyst having a Total Surface Area of 150 to 240 m2/g, a Total Pore Volume of 0.7 to 0.98 cc/g, and a Pore Diameter Distribution whereby less than about 20% of the Total Pore Volume is present as primary micropores of diameter less than about 100 Å, at least about 34% of the Total Pore Volume is present as secondary micropores of diameter of about 100 Å to 200 Å, and about 26 to 46% of the Total Pore Volume is present as mesopores of diameter greater than or equal to 200 Å.

A process for hydrotreating a charge hydrocarbon feed containing components boiling above 1000° F., and sediment-formers, sulfur, metals, asphaltenes, carbon residue, and nitrogen which comprises passing said charge hydrocarbon feed and hydrogen through a first ebullated bed reactor in liquid phase at a LHSV of 0.16 to 3.0 hr−1, at 650° F. to 850° F. and 1000 to 3500 psia, admitting hydrogen to said first ebullated bed reactor in amount of 2000 to 10,000 SCFB under isothermal hydrotreating conditions in the presence of a catalyst comprising a porous alumina support having incorporated therein about 1.1 to 6 wt. % of Group VIII metal oxide, and about 5 to 24 wt. % of a Group VI-B metal oxide, to provide a liquid and gaseous effluent containing a hydrotreated product,

• charging the liquid and gaseous effluent from said first ebullated bed reactor to a second reactor containing the same weight of catalyst as loaded into the first said reactor and which is operated at essentially the same pressure as the first reactor, but at a temperature about 0° to about 30° F. higher than the first said reactor to provide a second liquid effluent, and
• recovering said hydrotreated product containing a decreased content of components boiling above 1000° F., sediment, sulfur, metals, carbon residue, asphaltenes and
• said catalyst having been prepared by nulling a porous alumina powder with ammonium molybdate and nickel nitrate in the presence of an acid selected from the group consisting of phosphoric acid, nitric acid, and acetic acid to provide a mixture, extruding the mixture to form an extrudate, drying the extrudate and subjecting the dried extrudate to hydrothermal calcination to provide said catalyst,
• said catalyst having a Total Surface Area of 150 to 240 m2/g, a Total Pore Volume of 0.7 to 0.98 cc/g, and a Pore Diameter Distribution whereby less than about 20% of the Total Pore Volume is present as primary micropores of diameter less than about 100 Å, at least about 34% of the Total Pore Volume is present as secondary micropores of diameter of about 100 Å to 200 Å, and about 26 to 46% of the Total Pore Volume is present as mesopores of diameter greater than or equal to 200 Å.

A method of hydroprocessing a charge hydrocarbon feed containing components boiling above 1000°°F., and sulfur, metals, ad carbon residue, said process comprising:

• contacting said charge hydrocarbon feed with hydrogen at isothermal hydroprocessing conditions in the presence of a catalyst, said catalyst comprising 1.1 to 6 w % of a Group VIII metal oxide, 5 to 24 w % of a Group VIB metal oxide, and 0 to 2 w % of a phosphorus oxide, and wherein said catalyst is prepared by mulling the catalytic metals as salts with an alumina powder under acidic conditions to give an acidic mixture followed by extrusion of the acidic mixture and calcination in such a manner so that less Ban 5% of the Group VIII metal oxide contained in the catalyst is in an acid extractable form and wherein said catalyst has a Total Surface Area of 165 to 230 m2/g, a Total Pore Volume of 0.81 to 0.98 cc/g, and a Pore Diameter Distribution in which 22.0 to 36.0% of die Total Pore Volume is present as macropores of diameter greater than 250 Å, 64.0 to 78.0% of the Total Pore Volume is present as micropores of diameter less than 250 Å, greater than 60% of the incorporate volume is present as micropores of diameter 25 Å about a pore mode by volume of 100 to 120 Å, less than 0.05 cc/g of micropore volume is present in micropores with diameters less than 80 Å, thereby forming hydroprocessed product containing a decreased content of components boiling above 1000° F. and a decreased content of sulfur, metals, and carbon residue;
• and recovering said hydroprocessed product, the hydroprocessed product containing a decreased content of sediment in the portion of the hydroprocessed product boiling above 650° F.

A catalyst composition characterized by its ability to hydrotreat a charge hydrocarbon feed containing components boiling above 1000° F., and sediment-formers, sulfur, metals, asphaltenes, carbon residue, and nitrogen, said catalyst comprising comprising

• 1.1 to 6 w % of a Group VIII metal oxide,
• 5 to 24 w % of a Group VIB metal oxide, and
• 0 to 2 w % of a phosphorus oxide, and
• wherein said catalyst is prepared by mulling the catalytic metals as salts with an alumina powder under acidic conditions to give an acidic mixture followed by extrusion of the acidic mixture and calcination in such a manner so that less than 5% of the Group VIII metal oxide contained in the catalyst is in an acid extractable form and
• wherein said catalyst has a Total Surface Area of 165 to 230 m2/g, a Total Pore Volume of 0.81 to 0.98 cc/g, and a Pore Diameter Distribution in which 22.0 to 36.0% of the Total Pore Volume is present as macropores of diameter greater than 250 Å, 64.0 to 78.0% of the Total Pore Volume is present as micropores of diameter less than 250 Å, greater than 60% of the micropore volume is present as micropores of diameter 25 Å about a pore mode by volwme of 100 to 120 Å, less than 0.05 cc/g of rnicropore volume is present in inicropores with diameters less than 80 Å.