Pyrolysis of tobacco was studied in oxidative and nonoxidative (inert) environments at atmospheric pressure and temperatures ranging from 150 to 750 degrees C. The objective was to study the effect of pyrolysis conditions on the characteristics of the solid residue, i.e., char. The char was characterized using cross-polarization (13)C nuclear magnetic resonance (CPMAS NMR), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), the Brunauer-Emmett-Teller (BET) surface area, and the elemental composition. The char yield from pyrolysis (i.e., nonoxidative) decreased sharply with an increase in temperature to ca. 22% (dry, ash-free basis) at high temperatures. In oxidative pyrolysis, i.e., in 5% oxygen, the char was completely oxidized above 600 degrees C. The gaseous product from pyrolysis at high temperatures contained a significant concentration of hydrogen. The surface area of the char was low, with a maximum of 8 m(2)/g at 400 degrees C. SEM analysis indicated that pyrolysis of the tobacco led to a gradual accumulation of inorganic crystals on the exposed surfaces, and some constituents also melted, resulting in the formation of vesicles by evolving gas. NMR analysis showed significant changes in pectin and sugar constituents of the tobacco and breaking of glycosidic bonds of cellulose at 300-500 degrees C before the char became predominantly aromatic at high temperatures. FTIR results showed a continuous decrease in the intensity of the OH stretch with temperature and the aromatic character to be at maximum at 550-650 degrees C. The H/C ratio of the char decreased continuously with temperature, while the O/C ratio became constant above 300 degrees C due to the presence of oxides and carbonates in the char. The results are consistent with the analysis of the evolved gases.
Pyrolysis of chlorogenic acid was studied under varying conditions of temperature and reaction
environment. The objective was to study the effect of pyrolysis conditions on the composition of
the solid residue, i.e., char. Runs were made at atmospheric pressure under oxidative and non-oxidative (inert) atmospheres and at temperatures ranging from 250 to 750 °C. The characterization of char was done in terms of its elemental composition and surface area, and by Fourier
transform infrared (FTIR) and solid-state 13C nuclear magnetic resonance (NMR) spectroscopy.
The surface morphology of char was studied by scanning electron microscopy (SEM). The char
yield in non-oxidative runs decreased from 80% at 250 °C to 20% above 550 °C. In oxidative
runs, the char was completely oxidized at 550 °C. The surface area of char increased with
temperature to a maximum of 196 m2/g at 650 °C. SEM analysis indicated that the pyrolysis of
chlorogenic acid first formed a melt followed by formation of varying structures that decomposed
rapidly at high temperatures. The H/C and O/C ratios of the char decreased as the temperature
increased. NMR analysis showed that the resonance bands corresponding to carbonyl groups
mostly disappeared above 350 °C and the phenolic groups became almost totally absent in 650
°C char. The aromatic character of char was enhanced with increasing temperature. FTIR studies
indicated a gradual decrease in the intensities of OH and CO stretches at high temperatures.
At 750 °C, most bands disappeared, resulting in a char that was mainly an aromatic polymer of
carbon atoms. The oxidative pyrolysis enhanced mainly the surface area at the expense of char
yield. The results are consistent with the analysis of the evolved gases.
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