Abstract
Nitrogen-containing molecular sieves and nitrogen-containing carbon were
prepared and characterized by various spectroscopic tools such as powder
X-ray diffraction (XRD), N-2 adsorption-desorption isotherms, Fourier
transformed infra-red (FTIR) and Raman spectroscopy, scanning electron
microscopy (SEM), and X-ray photoelectron spectroscopy (XPS). The
catalytic properties of the solids exhibited different yields of ethyl
2-cyano-3-propylacrylate (ECPA) via Knoevenaguel reaction, according to
their amount of nitrogen incorporated to the solids. The influence of
reaction parameters such as the feed composition, temperature, type of
solvent and catalyst loading was also evaluated. It was shown that in
addition to the amount of nitrogen, the accessibility of the sites to
the reactants is a key factor for high catalytic activity. The best
conditions investigated for the production of ECPA were a BUT/ECA molar
ratio of 1 and a reaction time of 1 h at 30 degrees C. 50 mg of catalyst
is optimal for the reaction, but in general, the mass depends on other
parameters such as the amount of reactant. Characterisation of the spent
NC catalyst through BET surface area, GC-MS, SEM, Raman and infrared
spectroscopy indicated that the loss of nitrogen basic sites is the main
pathway for deactivation of the catalysts. (C) 2011 Elsevier B.V. All
rights reserved.
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