A technique for simultaneous in situ MAS NMR and on-line gas chromatographic studies of hydrocarbon conversions on solid catalysts under flow conditions
M. Hunger et al., A technique for simultaneous in situ MAS NMR and on-line gas chromatographic studies of hydrocarbon conversions on solid catalysts under flow conditions, CATAL LETT, 57(4), 1999, pp. 199-204
A new technique is introduced allowing simultaneous in situ MAS NMR investi
gations of hydrocarbon conversions on solids under flow conditions and on-l
ine gas chromatography. For adsorption of methanol on zeolite HBeta, equal
amounts of adsorbed molecules were determined by both analytical methods. S
tudying the synthesis of methyl tertiary-butyl ether (MTBE) on zeolite HBet
a using an MAS NMR rotor reactor, a constant yield of MTBE of Y-mtbe = 27%
was obtained up to a weight hourly space velocity of 1.4 h(-1). The variati
on of the reaction temperature led to a simultaneous change of the C-13 MAS
NMR signals of isobutoxy species and of the yield of MTBE determined by on
-line gas chromatography which indicates that isobutoxy species act as chem
ically active compounds. In this first application, the new in situ techniq
ue has demonstrated its advantage for a simultaneous investigation of compo
unds with a long residence time on the catalyst surface and of compounds ra
pidly leaving the catalyst surface.