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The local structure of non-porphyrin Ni and V in Maya residuum, hydrocracked residuum, and toluene-insoluble solid were determined by XAFS spectroscopy. In residuum, the first coordination shell of non-porphyrin V is similar to that for vanadyl tetraphenylporphyrin with four N at a distance of 2.08 A and one O at 1.67 A. Similarly, the first coordination shell of Ni non-porphyrin is similar to that in nickle tetraphenylporphyrin, i.e., four N at a distance of 1.90 A. The Ni and V coordination geometries are remarkably stable toward thermal cracking, catalytic hydrogen, and H2S. After hydrocracking to about 60% conversion of the residuum, the local coordination of Ni and V in the hydrocracked residuum is little changed. During hydrocracking, approximately 1% of the residuum is converted to toluene-insoluble solid, which contains high levels of Ni and V. Approximately 10% of the Ni and V in the solid is still present in a porphyrintype coordination geometry, while the remaining Ni and V has an octahedral coordination. In the latter, the V coordination contained one O at 1.64 A, four N at 2.14 A, and one N (or O) at 1.96 A, and the Ni coordination contained six N at 2.09 A. Ni or V sulfides are not formed in the toluene-insoluble solid.

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Structural Determination by XAFS Spectroscopy of Non-Porphyrin Nickel and Vanadium in Maya Residuum, Hydrocracked Residuum, and Toluene-Insoluble Solid