Characterization and degradation of lignin from steam explosion of pine and corn stalk of lignin: The role of superoxide ion and ozone

Steam explosion of corn stalk in the presence of 3% sulphuric acid at 200 °C for 5 min gave the highest recovery of lignin. Lignin has M_w = 2640 and M_z = 93,994. In the UV spectrum absorptions at λ = 231 and 280 nm were recorded. ¹H NMR spectrum of lignin showed signals attributable to cinnamaldehyde units, guaiacyl units, and syringyl units. Syringyl and guaiacyl units are in 1:1 ratio. ¹³C NMR spectrum showed signals for guaiacyl, syringyl, and p-hydroxyphenyl units. The spectrum showed a prevalence of guaiacyl units. The ¹³C NMR spectrum is in agreement with the presence of cinnamic units. The same characterization was performed on lignin from pine. The irradiation of lignin from pine from steam explosion process in the presence of oxygen, in conditions described for the formation of superoxide ion, for different irradiation time was followed isolating the lignin and determining the average molecular weight. The experiments showed that, until 8 h irradiation, M_n decreases, while M_w and M_z increases. After 8 h irradiation an inverse behaviour was observed, with an increase of M_n and a decrease of M_w and M_z. These results are in agreement with an initial polymerization process followed by a photoinduced degradation. Ozonization was carried out in acetonitrile–methanol solution. The reaction showed a zero-order kinetics. After 50 min the average molecular weight of lignin is the half. The reaction mixture was analyzed by using GC–MS. Oxalic acid was determined.