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Depozyty węglowe na katalizatorach i metody ich badania

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Góralski J. , Grams J. , Ludomirska I. , Paryjczak T. , Rzeźnicka I.

tom [Z] 54, 7-8

591-614

The reaction of organic compounds on solid catalysts can be accompanied by the formation of heavy by-products which can form a carbonaceous deposit on the surface and cause deactivation. Coke is an intractable, poorly defined material, changing in nature and composition with almost all possible reaction variables. Transmission electron microscopy (TEM) can be used to present coke directly, while electron loss spectroscopy (EELS) and X-ray photoelectron spectroscopy (XPS) can provide analytical and structural information. X-ray diffraction method (XRD)as well as 129XeNMR are the technique which can provide information about the location of the coke. Coke produces a decrease in catalytic activity by two mechanisms: active site suppression or pore blocking. The loss of sorption capacity of coked catalysts can help us to find out which deactivation mode has occurred. The technique of temperature programmed oxidation (TPO) with either evolved gas or gravimetric analysis (TGA) is often employed to investigate coke deposition on catalysts. Details of the proximity of coke to metal and nonmetal sites or the nature of coke are then inferred from the position of peaks in the resultant TPO profiles. The shape of these profiles can be affected by coke particle size and morphology. In recent years, 13C NMR in conjunction with proton cross-polarization (CP) and magic-angle spinning (MAS) has emerged as a powerful tool for studying the nature of coke formed during hydrocarbon conversion over catalysts. ]. IR spectroscopy has also been used to obtain information about the nature of the species present in the coke deposited on different zeolites as well as on other catalysts. The selective removal and transformation of carbonaceous compounds during reactivation were examined by means of IR combined with GC, TGA and NMR spectroscopy.