Gm. Robb et al., ACIDITY OF DEALUMINATED BETA-ZEOLITES VIA COUPLED NH3-STEPWISE TEMPERATURE-PROGRAMMED DESORPTION (STPD) AND FT-IR SPECTROSCOPY, MICROPOROUS AND MESOPOROUS MATERIALS, 20(4-6), 1998, pp. 307-316
Ammonia stepwise temperature programmed desorption (STPD) and FT-IR sp
ectroscopy have been used to study the acidity of dealuminated beta-ze
olites with Si/Al ratios in the range of 14.5 to 132. A carefully opti
mized temperature profile starting at 150 degrees C (in order to exclu
de physisorbed NH3) revealed five peaks at about 180 degrees C, 250 de
grees C, 350 degrees C, 440 degrees C, and 540 degrees C. Our investig
ations indicate that the first two peaks correspond to Lewis-type acid
ity of low strength and that the last three peaks correspond to Bronst
ed-type acidity of increasing strength. A one-to-one relation between
the total number of ammonia molecules desorbed in the above temperatur
e range and that of the Al atoms exists. High strength Lewis sites wer
e not observed probably because the extent of dehydroxylation in the a
bove temperature range was minimal. By increasing the level of dealumi
nation, it was found that the relative population of strong Bronsted s
ites increases in comparison with the weak ones. The present stepwise
temperature programmed desorption experiments coupled with FT-IR provi
de a very accurate tool for the quantitative measurement of the streng
th of the zeolite acid sites. (C) 1998 Elsevier Science B.V.