# US 4,392,985 A · Hydrocarbon conversion catalyst and method of preparation > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 4,392,985 A - Document ID: US4392985A - Status: Granted - Kind: A - Application number: 06/287,022 - Filed: 1981-07-27 - Granted: 1983-07-12 - Earliest claimed: 1981-07-27 - Assignees: Union Oil Company of California - Inventors: William S. Millman - Web page: https://patentgrep.com/patent/US4392985A ## CPC - C10G 45/08: in combination with chromium, molybdenum, or tungsten metals, or compounds thereof - B01J 27/188: with chromium, molybdenum, tungsten or polonium - C10G: CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION (cracking to hydrogen or synthesis gas C01B; cracking or pyrolysis of hydrocarbon gases to individual hydrocarbons or mixtures thereof of definite or specified constitution C07C; cracking to cokes C10B); RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES - B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS ## Abstract A hydrocarbon conversion catalyst containing cobalt and a Group VIB metal and having a substantially uniform cross-sectional phosphorus distribution is prepared by impregnating support particles with a solution containing dissolved cobalt, phosphorus, and at least 17 weight percent of Group VIB metal components, calculated as the trioxides, having a pH of less than 1.2, and characterized by an extincton coefficient in the ultraviolet spectrum of about 0.7.times.10.sup.4 to about 1.8.times.10.sup.4 liters/cm.moles of Group VIB metal, followed by aging, drying and calcining. The catalyst is useful for promoting a number of hydrocarbon conversion reactions, particularly those involving hydrogenative desulfurization. ## Claims ### Claim 1 A catalytic composition prepared by the method comprising the steps of (1) impregnating support particles with an aqueous impregnating solution comprising dissolved cobalt, phosphorus, and at least 17 weight percent of Group VIB metal components, calculated as the trioxides, and wherein said dissolved phosphorus, calculated as P, is in a weight ratio to the Group VIB metal trioxide of about 0.01 to about 0.5, said solution having a pH less than about 1.0 and being characterized by a maximum extinction coefficient in the ultraviolet spectrum of about 0.7.times.10.sup.4 to 1.8.times.10.sup.4 liters/cm.moles of Group VIB metal, and (2) activating the impregnated support particles. ### Claim 2 A catalytic composition prepared by the method comprising the steps of (1) impregnating support particles with an aqueous impregnating solution comprising dissolved cobalt, phosphorus, at least 17 weight percent of Group VIB metal components, calculated as the trioxides, and ammonium ions in a molar concentration greater than 1.5, said solution having a pH less than about 1.0, and wherein said dissolved phosphrous, calculated as P, is in a weight ratio to the Group VIB metal trioxide of about 0.01 to about 0.5, and (2) activating the impregnated support particles. ### Claim 3 (depends on 1) The composition defined in claim 1 wherein said solution further comprises ammonium ions having a molar concentration greater than 1.5. ### Claim 4 (depends on 1, 2) The composition defined in claim 1 or 2 wherein said aqueous solution comprises at least about 1 weight percent cobalt components, calculated as CoO, said Group VIB metal component comprises ammonium heptamolybdate and contains at least about 20 weight percent molybdenum components, calculated as MoO.sub.3, and said phosphorus is present in a form comprising orthophosphoric acid. ### Claim 5 (depends on 4) The composition defined in claim 4 wherein said solution comprises about 20 to about 25 weight percent molybdenum components, calculated as MoO.sub.3, and wherein said weight ratio of phosphorus to molybdenum components, calculated as MoO.sub.3, is about 0.05 to about 0.16. ### Claim 6 (depends on 4) The composition defined in claim 4 wherein said solution is further characterized by having a maximum absorbance in the range of about 1.3 to about 2.3 at a wave length in the range of about 200 to 210 nanometers when said solution is diluted such that the molar concentration of molybdenum (calculated as Mo) is in the range of about 0.7.times.10.sup.-4 to 3.3.times.10.sup.-4. ### Claim 7 (depends on 1, 2) The composition defined in claim 1 or 2 wherein said cobalt is selected from the group consisting of cobalt nitrate, cobalt oxide, and cobalt carbonate. ### Claim 8 A catalytic composition prepared by the method comprising the steps of (1) impregnating alumina-containing support particles with an aqueous impregnating solution comprising (a) at least one molybdenum compound selected from the group consisting of ammonium heptamolybdate, ammonium phosphomolybdate, and ammonium dimolybdate, (b) cobalt nitrate, and (c) orthophosphoric acid, and wherein said solution contains dissolved phosphorous, calculated as P, in a weight ratio to molybdenum trioxide of about 0.05 to about 0.2, said solution containing at least about 20 weight percent molybdenum components, calculated as MoO.sub.3, said solution having a pH less than about 1.0 and being characterized by an ultraviolet spectrum having a maximum absorbance in the range of about 1.3 to about 2.3 at a wavelength in the range of about 200 to about 210 nanometers when said solution is diluted such that the molar concentration of molybdenum (calculated as Mo) is in the range of about 0.7.times.10.sup.-4 to about 3.3.times.10.sup.-4, (2) aging said impregnated support particles, and (3) thermally activating said aged support particles. ### Claim 9 (depends on 8) The composition defined in claim 8 wherein said aged impregnated support particles are thermally activated by calcining said particles at a temperature of at least 750.degree. F. ### Claim 10 A method for preparing a catalyst comprising the steps of (1) impregnating support particles with an aqueous solution comprising dissolved cobalt, phosphorus, and at least 17 weight percent of Group VIB metal components, calculated as the trioxides, and wherein said dissolved phosphorus, calculated as P, is in a weight ratio to the Group VIB metal trioxide of about 0.01 to about 0.5, said solution having a pH less than about 1.0 and being characterized by a maximum extinction coefficient in the ultraviolet spectrum of about 0.7.times.10.sup.4 to 1.8.times.10.sup.4 liters/cm.moles of Group VIB metal, and (2) activating the impregnated support particles. ### Claim 11 (depends on 10) The method defined in claim 10 wherein said solution further comprises ammonium ions having a molar concentration greater than 1.5. ### Claim 12 (depends on 10) The method defined in claim 10 wherein prior to step (1) at least 30 percent of the pore volume of said support particles is filled with water. ### Claim 13 (depends on 10) The method defined in claim 10 wherein step (2) further comprises (a) aging said impregnated support particles, and (b) thermally activating said aged support particles. ### Claim 14 (depends on 10) The method defined in claim 10 wherein said phosphorus comprises orthophosphoric acid and said Group VIB metal compound is selected from the group consisting of ammonium heptamolybdate, ammonium phosphomolybdate, and ammonium dimolybdate. ### Claim 15 (depends on 10) The method defined in claim 10 wherein said cobalt is selected from the group consisting of cobalt nitrate, cobalt oxide, and cobalt carbonate. ### Claim 16 (depends on 10) The method defined in claim 10 further characterized by an ultraviolet spectrum having a maximum absorbance in the range of about 1.3 to about 2.3 at a wave length in the range of about 200 to about 210 nanometers. ### Claim 17 An impregnant solution for preparing hydrocarbon conversion catalysts comprising an aqueous solution comprising dissolved cobalt, phosphorus, and at least 17 weight percent of Group VIB metal components, calculated as the trioxides, and wherein said dissolved phosphorus, calculated as P, is in a weight ratio to the Group VIB metal trioxide of about 0.1 to about 0.5, said solution has a pH less than about 1.0 and is characterized by a maximum extinction coefficient in the ultraviolet spectrum of about 0.7.times.10.sup.4 to 1.8.times.10.sup.4 liters/cm.moles of Group VIB metal. ### Claim 18 An impregnant solution for preparing hydrocarbon conversion catalysts comprising an aqueous solution comprising dissolved phosphorus, at least 20 weight percent of Group VIB metal components, calculated as the trioxides, and a cobalt compound, soluble in acidic aqueous solution, and wherein said dissolved phosphorus, calculated as P, is in a weight ratio to the Group VIB metal of about 0.03 to about 0.40, said solution has a pH less than about 1.0 and is characterized by an ultraviolet spectrum having a maximum absorbance in the range of about 1.3 to about 2.3 at a wavelength in the range of about 200 to 210 nanometers and a maximum extinction coefficient of about 1.10.times.10.sup.4 to 1.4.times.10.sup.4 liters/cm.moles of Group VIB metal. ### Claim 19 (depends on 17, 18) The solution defined in claim 17 or 18 further comprising ammonium ions having a molar concentration greater than 1.5. ### Claim 20 (depends on 17, 18) The solution defined in claim 17 or 18 wherein said phosphorus is present in a form comprising orthophosphoric acid and said Group VIB metal component is selected from the group consisting of ammonium heptamolybdate, ammonium phosphomolybdate, and ammonium dimolybdate. ### Claim 21 (depends on 17, 18) The solution defined in claim 17 or 18 wherein said cobalt is selected from the group consisting of cobalt nitrate, cobalt oxide, and cobalt carbonate.