Articles | Volume 4, issue 1
Regular research article
13 Apr 2015
Regular research article |  | 13 Apr 2015

Is it possible to detect in situ the sulfur loading of a fixed bed catalysts with a sensor?

P. Fremerey, A. Jess, and R. Moos

Abstract. This study reports on a sensor concept to measure in situ sulfur poisoning (sulfidation) of refinery catalysts, in this case, of commercial silica pellets loaded with highly dispersed nickel. Catalyst pellets were poisoned in diluted H2S between 100 and 400 °C and the sulfidation of the catalyst was observed. During this process, nickel sulfides are formed on the catalyst according to X-ray diffraction spectra and energy dispersive X-ray spectroscopy data. The sulfidation kinetics was quantitatively described by a shrinking core model. Representative catalyst pellets were electrically contacted, and their impedance was recorded in situ during sulfidation. At the beginning, the particles are highly insulating and behave capacitively. Their conductivity increases by decades during sulfidation. At high temperatures, an almost constant slope in the double-logarithmic representation vs. time can be found. At low temperatures, the conductivity remains constantly low for a long time but changes then rapidly by decades, which is also indicated by the phase that drops from capacitive to ohmic behavior. Since nickel sulfides exhibit a lower conductivity than nickel, the conductivity increase by decades during sulfidation can only be explained by electrically conducting percolation paths that form during sulfidation. They originate from the increased volume of sulfides compared to the pure nickel metal.

Short summary
A concept to measure in situ sulfidation of silica pellet catalysts loaded with nickel is evaluated. During sulfidation between 100 and 400°C nickel sulfides form. The electrical impedance of the pellets was recorded in situ. At first, the particles are highly insulating but during sulfidation their conductivity increases by decades. Since nickel sulfides are less conductive than nickel, the strong conductivity increase may be due to conducting percolation paths that form during sulfidation.