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- Delignification of Cistus ladanifer Biomass by Organosolv and Alkali ProcessesPublication . Alves Ferreira Caturra, Júnia Aparecida; Lourenço, Ana; Morgado, Francisca; Duarte, Luís C.; Roseiro, Luisa B.; Fernandes, M. C.; Pereira, Helena; Carvalheiro, FlorbelaABSTRACT: Residues of Cistus ladanifer obtained after commercial steam distillation for essential oil production were evaluated to produce cellulose enriched solids and added-value lignin-derived compounds. The delignification of extracted (CLRext) and extracted and hydrothermally pretreated biomass (CLRtreat) was studied using two organosolv processes, ethanol/water mixtures (EO), and alkali-catalyzed glycerol (AGO), and by an alkali (sodium hydroxide) process (ASP) under different reaction conditions. The phenolic composition of soluble lignin was determined by capillary zone electrophoresis and by Py-GC/MS, which was also used to establish the monomeric composition of both the delignified solids and isolated lignin. The enzymatic saccharification of the delignified solids was also evaluated. The ASP (4% NaOH, 2 h) lead to both the highest delignification and enzymatic saccharification (87% and 79%, respectively). A delignification of 76% and enzymatic hydrolysis yields of 72% were obtained for AGO (4% NaOH) while EO processes led to lower delignification (maximum lignin removal 29%). The residual lignin in the delignified solids were enriched in G- and H-units, with S-units being preferentially removed. The main phenolics present in the ASP and AGO liquors were vanillic acid and epicatechin, while gallic acid was the main phenolic in the EO liquors. The results showed that C. ladanifer residues can be a biomass source for the production of lignin-derivatives and glucan-rich solids to be further used in bioconversion processes.
- Chemical composition and structural features of cellolignin from steam explosion followed by enzymatic hydrolysis of Eucalyptus globulus barkPublication . Magina, Sandra; Marques, Susana; Gírio, Francisco; Lourenço, Ana; Barros-Timmons, Ana; Evtuguin, Dmitry V.ABSTRACT: Bark is one of the main wastes of the chemical and mechanical processing of Eucalyptus globulus wood. The proposed biochemical processing of bark via saccharification pathway involves steam explosion (SE) pretreatment (severity factor log R0 of 4.22) followed by enzymatic hydrolysis using an enzymatic cocktail composed of cellulolytic and xylanolytic enzymes. Almost 70% cellulose saccharification was achieved. The remaining cellolignin residue (CLEZ) was analysed for its chemical composition and structural features by conventional wet chemistry methods and a series of spectroscopic tools (FTIR-ATR, solid-state CP/MAS C-13 NMR spectroscopy and wide-angle X-ray scattering (WAXS)). The main CLEZ component (about 51%) is acid-insoluble lignin, the chemical composition of which in terms of the ratio of syringyl (S), guaiacyl (G) and p-hydroxyphenyl (H) units (70:28:2) is very close to that in the initial bark. This lignin is highly condensed and structurally associated with condensed tannins, which makes CLEZ recalcitrant to delignification by common methods. About one third of cellulose in eucalyptus bark after SE was inaccessible to enzymatic hydrolysis and remained in the CLEZ. This cellulose, structurally similar to microcrystalline cellulose, is imbedded into the lignin-tannins condensed matrix and extremely difficult to purify. In contrast to cellulose, bark hemicelluloses were effectively removed in enzymatic hydrolysis, with only small amounts (<2%) remaining in CLEZ. Among other CLEZ ingredients, proteins and inorganic/organic salts were the most abundant. The latter includes noticeable amounts of calcium oxalate phytoliths (up to 9%), Fe and Si salts. The eventual application areas of CLEZ are discussed.