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Issue 12, 2004
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The production of nicotineamide during the thermal desorption of 3-cyanopyridine (3CYP) from Ni2+- and Al3+- exchanged bentonite. A TG-MS, variable temperature DRIFTS and XRD study

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Abstract

Samples of air-dried and heated Ni2+- and Al3+-exchanged bentonite (SWy-2) have been exposed to 3-cyanopyridine (3CYP) vapour for six days. The resulting intercalates were studied using variable temperature XRD, DRIFTS, thermogravimetry (TG) and TG-MS. The amount of water co-adsorbed with 3CYP did not influence the initial 13.2 Å spacing of the Al3+-complex but the d-spacing of the heated Ni2+-sample was ca. 5 Å less that the 21.5 Å spacing of its air-dried counterpart. This difference in layer spacings suggests that 3CYP adopts an arrangement in which the plane of the aromatic ring is parallel with the aluminosilicate layer in the Al3+-clay whereas in the Ni2+-form the plane of the ring is perpendicular to the clay surface. TG-MS confirmed that 3CYP and water were the major species desorbed from all samples and that the contraction in the d-spacing upon heating the Ni2+-3CYP complex arose from loss of these species. The appearance of a band near 1680 cm−1 in the VT-DRIFTS spectra at temperatures above 150 °C indicated the formation of amide(s). Correlation with TG-MS data confirmed the transformation of small quantities of 3CYP to nicotinamide. Some 3CYP was protonated in the Al3+-samples.

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Publication details

The article was received on 25 Feb 2004, accepted on 23 Apr 2004 and first published on 12 May 2004


Article type: Paper
DOI: 10.1039/B402934H
Citation: Phys. Chem. Chem. Phys., 2004,6, 3184-3191
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    The production of nicotineamide during the thermal desorption of 3-cyanopyridine (3CYP) from Ni2+- and Al3+- exchanged bentonite. A TG-MS, variable temperature DRIFTS and XRD study

    J. Forsyth, C. Breen, T. Hughes and J. Yarwood, Phys. Chem. Chem. Phys., 2004, 6, 3184
    DOI: 10.1039/B402934H

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