# US 5,707,921 A · Method of preparing isomerization catalyst composition > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 5,707,921 A - Document ID: US5707921A - Status: Granted - Kind: A - Application number: 08/529,179 - Filed: 1995-09-15 - Granted: 1998-01-13 - Earliest claimed: 1995-09-15 - Assignees: Phillips Petroleum Company - Inventors: An-hsiang Wu; Charles A. Drake; Ralph J. Melton - Web page: https://patentgrep.com/patent/US5707921A ## CPC - B01J 37/22: Halogenating - B01J 27/125: with scandium, yttrium, aluminium, gallium, indium or thallium - B01J 27/13: Platinum group metals - B01J 37/04: Mixing {(B01J37/0009, B01J37/0018 take precedence)} - C07C 5/2791: {with metals} - C07C 2521/04: Alumina - C07C 2523/42: Platinum - C07C 2523/44: Palladium - C07C 2523/755: Nickel - C07C 2527/126: Aluminium chloride - B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS - C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS ## Abstract A Group VIII metal- and chloride-containing composition (effective as an alkane/cycloalkane isomerization catalyst) is prepared by a method which comprises mixing at least one aluminum- and chlorine-containing compound (preferably AlCl.sub.3) with a solid material containing at least one Group VIII metal (Pt and/or Pd and/or Ni) and alumina, heating the obtained solid mixture in an inert gas, and then treating the solid mixture with a gas mixture comprising hydrogen gas and HCl and/or chloroalkane (such as CCl.sub.4). ## Claims ### Claim 1 A method of preparing a solid Group VIII metal-and chlorine-containing composition which comprises: (1) mixing at least one aluminum-and chlorine-containing compound selected from the group consisting of aluminum chloride and alkyl aluminum chlorides with a solid material which comprises (I) at least one Group VIII metal selected from the group consisting of platinum, palladium and nickel and (ii) alumina as the support, wherein said solid material has been prepared by a method comprising: (a) impregnating an alumina material with at least one compound of a Group VIII metal selected from the group consisting of platinum, palladium and nickel; (b) calcining the impregnated alumina obtained in step (a) at a temperature of about 300.degree.-650.degree. C. for a time period of at least about 10 minutes; and (c) treating the calcined material obtained in step (b) with a reducing gas comprising free hydrogen at a temperature of about 200.degree.-550.degree. C. for a time period of at least about 10 minutes, and wherein the weight ratio of said at least one aluminum- and chlorine-containing compound to said solid material used in step (1) is in the range of about 0.05:1 to about 1:1; (2) heating the mixture obtained in step (1) in a substantially inert gas atmosphere at a temperature of about 450.degree.-700.degree. C. for a time period of at least about 10 minutes; and (3) treating the material obtained in step (2) with a gas mixture comprising hydrogen gas and at least one chlorine-containing compound selected from the group consisting of hydrogen chloride and chloroalkanes, at a temperature of about 50.degree.-700.degree. C. for a time period of at least about 10 minutes. ### Claim 2 (depends on 1) A method in accordance with claim 1, wherein said aluminum- and chlorine-containing compound used in step (1) is selected from the group consisting of methylaluminum dichloride, methylaluminum sesquichloride, dimethylaluminum chloride, ethylaluminum dichloride, ethylaluminum sesquichloride, diethylaluminum chloride, propylaluminum dichloride, dipropylaluminum chloride, butylaluminum dichloride, dibutylaluminum chloride and mixtures thereof. ### Claim 3 (depends on 1) A method in accordance with claim 1, wherein said at least one aluminum- and chlorine-containing compound is aluminum chloride. ### Claim 4 (depends on 3) A method in accordance with claim 3, wherein the time period of step (2) is about 0.5-20 hours, the molar ratio of hydrogen to said at least one chlorine-containing compound in said gas mixture used in step (3) is about 0.01:1 to about 100:1, and the time period of step (3) is about 0.2-20 hours. ### Claim 5 (depends on 4) A method in accordance with claim 4, wherein said at least one chlorine-containing compound used in step (3) is selected from the group consisting of hydrogen chloride and chloroalkanes containing 1-4 carbon atoms per molecule and 1-6 chlorine atoms per molecule. ### Claim 6 (depends on 5) A method in accordance with claim 5, wherein the temperature in step (2) is about 625.degree.-675.degree. C., the time period of step (2) is about 0.5-2 hours, the molar ratio of hydrogen to said at least one chlorine-containing compound used in step (3) is about 0.05:1 to about 50:1, the temperature in step (3) is about 150.degree.-400.degree. C., and the time period of step (3) is about 0.5-2 hours. ### Claim 7 (depends on 6) A method in accordance with claim 6, where said at least one chlorine-containing compound used in step (3) is selected from the group, consisting of hydrogen chloride and carbon tetrachloride. ### Claim 8 (depends on 7) A method in accordance with claim 7, wherein the molar ratio of hydrogen to said at least one chlorine-containing compound used in step (3) is about 0.2:1 to about 20:1 and the temperature in step (3) is about 180.degree.-280.degree. C. ### Claim 9 (depends on 1) A method in accordance with claim 1, wherein at least one titanium compound is also present in step (1). ### Claim 10 (depends on 1) A method in accordance with claim 1, wherein step (b) is carried out for a time period of about 0.5-20 hours, and step (c) is carried out for a time period of about 0.5-20 hours. ### Claim 11 (depends on 1) A method in accordance with claim 1, wherein step (a) is carried out with at least one dissolved platinum compound. ### Claim 12 (depends on 11) A method in accordance with claim 11, wherein said alumina material is also impregnated with at least one dissolved titanium compound. ### Claim 13 (depends on 1) A method in accordance with claim 1, wherein step (a) is carried out with at least one dissolved palladium compound. ### Claim 14 (depends on 1) A method in accordance with claim 1, wherein step (a) is carried out with at least one dissolved nickel compound. ### Claim 15 (depends on 1) A method in accordance with claim 1, wherein the material obtained in step (3) comprises about 0.1-8 weight-% of said at least one Group VIII metal and about 2-7 weight-% chlorine. ### Claim 16 (depends on 15) A method in accordance with claim 15, wherein said at least one Group VIII metal is platinum. ### Claim 17 (depends on 15) A method in accordance with claim 15, wherein said at least one Group VIII metal is palladium. ### Claim 18 (depends on 15) A method in accordance with claim 15, wherein said at least one Group VIII metal is nickel. ### Claim 19 (depends on 15) A method in accordance with claim 15, wherein said material obtained in step (3) additionally comprises about 0.05-1 weight-% titanium.