The United States of America As Represented by the United States

Iowa State University Research Foundation Inc

University of Delaware

Glenn L Schrader

Kwan F Koo

Alvin B Stiles

Kevin F McCarty

Irmgard M Schewe-Miller

Shane J Hilsenbeck

Xiaobing Xie

Robert E McCarley

New amorphous molybdenum/tungsten sulfides with the general formula M.sup.n+.sub.2x/n (L.sub.6 S.sub.8)S.sub.x, where L is molybdenum or tungsten and M is a ternary metal, has been developed. Characterization of these amorphous materials by chemical and spectroscopic methods (IR, Raman, PES) shows that the (M.sub.6 S.sub.8).sup.0 cluster units are present. Vacuum thermolysis of the amorphous Na.sub.2x (Mo.sub.6 S.sub.8)S.sub.x .multidot.yMeOH first produces poorly crystalline NaMo.sub.6 S.sub.8 by disproportionation at 800.degree. C. and well-crystallized NaMo.sub.6 S.sub.8 at .gtoreq. 900.degree. C. Ion-exchange of the sodium material in methanol with soluble M.sup.2+ and M.sup.3+ salts (M=Sn, Co, Ni, Pb, La, Ho) produces the M.sup.n+.sub.2x/n (Mo.sub.6 S.sub.8)S.sub.x .multidot.yMeOH compounds. Additionally, the new reduced ternary molybdenum sulfides with the general formula M.sup.n+.sub.2x/n Mo.sub.6 S.sub.8+x (MeOH).sub.y �MMOS! (M=Sn, Co, Ni) is an effective hydrodesulfurization (HDS) catalyst both as-prepared and after a variety of pretreatment conditions. Under specified pretreatment conditions with flowing hydrogen gas, the SnMoS type catalyst can be stabilized, and while still amorphous, can be considered as 'Chevrel phase-like' in that both contain Mo.sub.6 S.sub.8 cluster units. Furthermore, the small cation NiMoS and CoMoS type pretreated catalyst showed to be very active HDS catalysts with rates that exceeded the model unpromoted and cobalt-promoted MoS.sub.2 catalysts.

Reduced ternary molybdenum and tungsten sulfides and hydroprocessing

A method is provided to form a lead Chevrel phase coating of the formula PbMo.sub.6 S.sub.8 on a substrate by employing the techniques of reactive sputtering comprising: (a) sputtering lead (Pb) and molybdenum (Mo) from homogeneous targets of Pb and Mo in vacuo in an atmosphere of argon and hydrogen sulfide so as to deposit a coating of PbMo.sub.6 S.sub.8 on said substrate; and (b) annealing said PbMo.sub.6 S.sub.8 coating at a pressure at which Pb is not lost from the coating; wherein the targets and the substrate are contained within a vacuum chamber during steps (a) and (b).

Reactive sputter deposition of lead chevrel phase thin films

A method is provided to form a basal oriented coating of molybdenum sulfide of the formula MoS.sub.2 on a substrate by employing the techniques of reactive sputtering comprising: (a)(i) sputtering lead (Pb) and molybdenum (Mo) from homogeneous targets of Pb and Mo in vacuo in an atmosphere of argon and hydrogen sulfide or (ii) sputtering Pb and MoS.sub.2 from homogeneous targets of Pb and MoS.sub.2 in an atmosphere of argon (no H.sub.2 S), so as to deposit a coating comprising of Pb, S and Mo on said substrate; and (b) annealing said coating at a pressure at which the Pb is lost from the coating; wherein the targets and the substrate are contained within a vacuum chamber during steps (a) and (b).

Method for preparing basal oriented molybdenum disulfide (MoS.sub.2)

A process is disclosed for the hydrodesulfurization of sulfur-containing hydrocarbon fuel with reduced ternary molybdenum sulfides, known as Chevrel phase compounds. Chevrel phase compounds of the general composition M.sub.x Mo.sub.6 S.sub.8, with M being Ho, Pb, Sn, Ag, In, Cu, Fe, Ni, or Co, were found to have hydrodesulfurization activities comparable to model unpromoted and cobalt-promoted MoS.sub.2 catalysts. The most active catalysts were the 'large' cation compounds (Ho, Pb, Sn), and the least active catalysts were the 'small' cation compounds (Cu, Fe, Ni, Co.).

Hydrodesulfurization catalysis by Chevrel phase compounds

A catalyst for the manufacture of organic compounds comprising an intimate mixture of a reducible metal oxide and at least one refractory oxide, treated by heating to a temperature in the range of 550.degree. C. to 1000.degree. C. in the presence of a preselected reducing gas in amount sufficient to substantially inhibit or disrupt crystallite growth as evidenced by characteristic x-ray diffraction pattern, concomitantly enhancing catalytic activity, and the method of preparation.

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Ames, IA, United States of America

Glenn L Schrader