STUDIES ON DEPOSITS OF SPENT HYDRO-TREATING CATALYST: A STUDY BY COMBINED ANALYTICAL TECHNIQUES

Abstract

ABSTRACT Carbonaceous and non-carbonaceous deposits on a Ni-Mo catalyst, stemming from atmospheric residue upgrading in an ARDS unit were subjected to a combination of analytical techniques, i.e. SF extraction, TGA/DTA/MS, DRIFT, l3C CP-MAS NMR, XRD and elemental analysis. Since the spectroscopic features of several components of the deposit interfere with each other a detailed deposit characterization was only achieved by stepwise removal of certain components by SFE deoiling and calcination. SF extraction stripped about 22 wt % of the carbonaceous deposit of the spent catalyst increasing the sp2/(sp3 + sp2) ratio of the NMR-visible carbon from 0 63 to 0.67. TGA revealed three separate temperature ramps for stepwise driving off of deposited material- first ramp, 30° C - 280° C, loss of oil and sulfur from metal sulfides; second ramp, 280° C - 450° C, loss of carbonaceous material like coke; third ramp, 500° C - 680° C, loss of metal sulfates. Further calcination up to 1000° C has no effect on the metal content of the deposition but transforms the framework γ-Al2O3 into α-Al2O3. Entire burn-off of