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- Avaliação do potencial de valorização de sobrantes agroflorestais por um processo organosolv baseado em propilenoglicolPublication . Sampaio, Bruno; Pinto, Filomena; Carvalheiro, Florbela; Duarte, Luís C.RESUMO: Os processos de fracionamento da biomassa são ainda responsáveis por uma parcela substancial dos custos de operação das biorrefinarias, tendo também um impacto muito significativo no desempenho ambiental, pelo que são considerados uma etapa chave para aumentar a competitividade destas instalações industriais. Neste trabalho propõe-se um processo organosolv inovador, baseado em propilenoglicol (PG) um solvente alternativo, não-inflamável, não-tóxico, e que apresenta uma reduzida pressão de vapor, o que permite a operação a pressões próximas da atmosférica, mesmo a temperaturas moderadamente elevadas (até aproximadamente 190ºC). Os resultados obtidos permitem confirmar o elevado potencial do processo organosolv com PG para a desconstrução da palha de trigo, com as vantagens de apresentar uma operação mais segura e económica em comparação com a utilização dos solventes convencionais. São também apresentados e discutidos quais os caminhos mais adequados para a intensificação do processo.
- Métodos de fraccionamento de biomassa para as biorrefinariasPublication . Carvalheiro, Florbela; Duarte, Luís C.; Lukasik, Rafal M.; Moniz, PatriciaO desenvolvimento de processos que permitam o fraccionamento eficiente da biomassa (tradicionalmente designados por pré-tratamentos) constitui uma parte muito significativa do esforço científico que tem sido feito para a transformação das biorrefinarias numa realidade industrial. Este artigo apresenta uma breve revisão dos processos de fraccionamento, sendo dada particular atenção a processos emergentes, discutindo também as suas possíveis vantagens e limitações.
- Hydrothermal pretreatment of several lignocellulosic mixtures containing wheat straw and two hardwood residues available in Southern EuropePublication . Silva-Fernandes, Talita; Duarte, Luís C.; Carvalheiro, Florbela; Loureiro-Dias, M. Conceição; Fonseca, César; Gírio, FranciscoThis work studied the processing of biomass mixtures containing three lignocellulosic materials largely available in Southern Europe, eucalyptus residues (ER), wheat straw (WS) and olive tree pruning (OP). The mixtures were chemically characterized, and their pretreatment, by autohydrolysis, evaluated within a severity factor (log R0) ranging from 1.73 up to 4.24. A simple modeling strategy was used to optimize the autohydrolysis conditions based on the chemical characterization of the liquid fraction. The solid fraction was characterized to quantify the polysaccharide and lignin content. The pretreatment conditions for maximal saccharides recovery in the liquid fraction were at a severity range (log R0) of 3.65–3.72, independently of the mixture tested, which suggests that autohydrolysis can effectively process mixtures of lignocellulosic materials for further biochemical conversion processes.
- Deconstruction of the hemicellulose fraction from lignocellulosic materials into simple sugarsPublication . Gírio, Francisco; Carvalheiro, Florbela; Duarte, Luís C.; Lukasik, Rafal M.Hemicelluloses hold a great promise for the production of added-value compounds in the biorefinery framework. Specifically, the xylan-rich hemicelluloses from hardwoods and agro-industrial residues present themselves as effective feedstock choices for the biotechnological production of xylitol. This paper reviews the various hemicellulose structures present in such materials and critically evaluates the available processing options to produce xylose-rich fermentable hydrolysates. Currently, acid-based processes still present the best trade-off between operation easiness and xylose yield and recovery. Nevertheless, concerns regarding the impact of the fractionation processes on the overall upgradability of all biomass fractions (namely, cellulose and specially lignin) may turn the route to other strategies. Specifically, the combined/sequential use of processes targeting hemicellulose dissolution and hydrolysis might hold great promise for the economical production of pentoses.
- Production of liquid compounds by co-pyrolysis of different pre-treated biomasses mixed with plastic wastesPublication . Pinto, Filomena; Duarte, Luís C.; Carvalheiro, Florbela; Paradela, Filipe; Costa, Paula; Marques, Joana; Andre, Rui N.; Marques, Paula; Costa, Diogo; Sampaio, BrunoABSTRACT: As an innovation to conventional biomass pyrolysis to produce liquid biofuels, different types of biomass wastes were pre-treated by autohydrolysis, prior to pyrolysis. Eucalyptus forestry waste, corn cobs agricultural residue, and miscanthus (an energy crop) were autohydrolysed. Autohydrolysis led to valuable sugar-rich stream that may be used in fermentation and to solids rich in lignin that were pyrolysed. Pyrolysis of autohydrolysed eucalyptus led to an increase in liquids yields of 24 % in relation to untreated eucalyptus, as autohydrolysis weakened initial macromolecular structure and thus helped chemical bonds breakdown during pyrolysis. However, similar pyrolysis liquid yields were obtained by autohydrolysed or untreated corn cobs and miscanthus, thus feedstock composition is an important issue. Nevertheless, the production of added value products by autohydrolysis may still justify this pre-treatment. Otherwise, more severe pre-treatments of these biomasses might improve co-pyrolysis as it happened with eucalyptus. As polyethylene (PE) is easier to pyrolyse than biomass and greatly favours the production of liquid hydrocarbons, autohydrolysed and untreated biomass was mixed with PE wastes to be used in co-pyrolysis. The rise of PE content in the blend clearly favoured the production of liquid products of pre-treated and untreated biomass. 75 %wt. of PE in the blend led to liquid yields of 72 %wt. for untreated eucalyptus and of 82 %wt. for autohydrolysed eucalyptus.
- Recovery of bioactive compounds from industrial exhausted olive pomace through ultrasound-assisted extractionPublication . Gómez Cruz, Irene; Contreras, Maria del Mar; Carvalheiro, Florbela; Duarte, Luís C.; Roseiro, Luisa B.; Romero, Inmaculada; Castro, EulogioABSTRACT: Simple Summary Exhausted olive pomace (EOP) is the main residue of the pomace oil extraction industry, which is generated in large quantities and has limited applications. Thus, this study aimed to obtain bioactive compounds from EOP using ultrasound-assisted extraction as a potential first valorization step. Two types of devices were tested: bath- and probe-type UAE. The operational parameters were studied and optimized to maximize the antioxidant compounds. In particular, hydroxytyrosol was the main phenolic compound identified and its content was 5.16 mg/g EOP (bath-type UAE) and 4.96 mg/g EOP (probe-type UAE). Mannitol was also detected in the extract, 59.53 mg/g EOP (bath-type UAE) and 69.73 mg/g EOP (probe-type UAE). The results highlight the great potential EOP has as a source of bioactive compounds, with applicability in several sectors. Moreover, the probe-type UAE shows potential to be applied for obtaining these bioactive compounds in a continuous and faster manner. Exhausted olive pomace (EOP) is the main agro-industrial waste of the olive pomace extracting industries. It contains phenolic compounds and mannitol, so the extraction of these bioactive compounds should be considered as a first valorization step, especially if EOP is used as biofuel. Therefore, EOP was subjected to bath-type ultrasound-assisted extraction (UAE), and the effects of the acetone concentration (20-80%, v/v), solid load (2-15%, w/v), and extraction time (10-60 min) on the extraction of antioxidant compounds were evaluated according to a Box-Behnken experimental design. By means of the response surface methodology, the optimum conditions were obtained: 40% acetone, 8.6% solids, and 43 min. For all the extracts, the total phenolic content (TPC), flavonoid content (TFC), and antioxidant activity (DPPH, ABTS, and FRAP) were determined. With the aim of shortening the extraction time, a two-level factorial experiment design was also carried out using a probe-type UAE, keeping the solid load at 8.6% (w/v) and the acetone concentration at 40% (v/v), while the amplitude (30-70%) and the extraction time (2-12 min) were varied to maximize the aforementioned parameters. Finally, a maximum of phenolic compounds was reached (45.41 mg GAE/g EOP) at 12 min and 70% amplitude. It was comparable to that value obtained in the ultrasonic bath (42.05 mg GAE/g EOP), but, remarkably, the extraction time was shortened, which translates into lower costs at industrial scale. Moreover, the bioactive compound hydroxytyrosol was found to be the major phenolic compound in the extract, i.e., 5.16 mg/g EOP (bath-type UAE) and 4.96 mg/g EOP (probe-type UAE). Other minor phenolic compounds could be detected by capillary zone electrophoresis and liquid-chromatography-mass spectrometry. The sugar alcohol mannitol, another bioactive compound, was also found in the extract, and its content was determined. Thus, the use of this technology can support the valorization of this waste to obtain bioactive compounds, including mannitol, hydroxytyrosol, and other derivatives, before being applied for other uses.
- Hydrothermal processing of hardwoods and agro-industrial residues :evaluation of xylo-oligosaccharides productionPublication . Carvalheiro, Florbela; Fernandes, Talita Silva; Duarte, Luís C.; Lopes, Sónia; Moura, Patrícia; Pereira, Helena; Gírio, FranciscoAutohydrolysis was used as a pre-treatment method for the selective hydrolysis of hemicelluloses of four lignocellulosic materials: eucalypt wood chips (EWC), corn cobs (CC), wheat straw (WS) and brewery’s spent grain (BSG), and the process was optimized towards the production of xylo-oligosaccharides (XOS). The effects of temperature, both at isothermal (150-190ºC), and non-isothermal (up to 240ºC) conditions, and liquid-to-solid ratio (LSR), 8 or 10 g/g, on the composition of both the liquid and solid phases were studied. The operational conditions leading to the maximal recovery of XOS for each raw material were established and discussed based on the severity factor (log R0). The higher yields obtained were in the range of 43–65% of the feedstock (arabino)xylan, with the highest value attained for CC for log R0 =3.75. Under the optimised conditions for XOS production, glucan was only slightly solubilised, enabling an enrichment of the solid phase (up to 67% of glucan for EWC). Delignification was also not extensive reaching utmost 18%, in the case of CC. cosmetic industries.
- Green Fractionation Approaches for the Integrated Upgrade of Corn CobsPublication . Fialho, João; Moniz, Patricia; Duarte, Luís C.; Carvalheiro, FlorbelaABSTRACT: Corn cob is an abundant agricultural residue worldwide, with high potential and interesting composition, and its valorization still needs to be studied. Selectively fractionating its structural components (hemicellulose, cellulose, and lignin), value-added products can be produced, eliminating waste. In this work, integrated fractionation approaches were developed and evaluated. First, an organosolv process was optimized (ethanol:water, 50:50, w/w). Then, as a comparative method, alkaline delignification (using NaOH, 1-2%) was also studied. The organosolv process allowed a significant delignification of the material (79% delignification yield) and, at the same time, a liquid phase containing a relevant concentration (14.6 g/L) of xylooligosaccharides (XOS). The resulting solid fraction, rich in cellulose, showed an enzymatic digestibility of 90%. The alkaline process increased the delignification yield to 94%, producing a solid fraction with a cellulose enzymatic digestibility of 83%. The two later techniques were also used in a combined strategy of hydrothermal processing (autohydrolysis) followed by delignification. The first allowed the selective hydrolysis of hemicellulose to produce XOS-rich hydrolysates (26.8 g/L, 67.3 g/100 g initial xylan). The further delignification processes, alkaline or organosolv, led to global delignification yields of 76% and 93%, respectively. The solid residue, enriched in glucan (above 75% for both combined processes), also presented high enzymatic saccharification yields, 89% and 90%, respectively. The fractionation strategies proposed, and the results obtained are very promising, enabling the integrated upgrading of this material into a biorefinery framework.
- Distillery residues from Cistus ladanifer (Rockrose) as feedstock for the production of added-value phenolic compounds and hemicellulosic oligosaccharidesPublication . Alves Ferreira Caturra, Júnia Aparecida; Duarte, Luís C.; Lourenço, Ana; Roseiro, Luisa B.; C. Fernandes, M.; Pereira, Helena; Carvalheiro, FlorbelaABSTRACT: Cistus ladanifer residues obtained after essential oil distillation were extracted with ethanol and water (CLRext) and subsequently hydrothermally treated (autohydrolysis) in order to selectively hydrolyze hemicelluloses. The extraction removed a significant amount of potentially valuable compounds (40% w/w, dry basis), foremost, phenolic compounds (0.363 and 0.250 g gallic acid equivalent/g extract, respectively, for water and ethanol). Autohydrolysis was studied under diverse severity factors (log R-o), in the temperature range of 150 to 230 degrees C. The hydrolyzates mainly contain oligosaccharides, reaching the highest concentration (23.5g/L) for log R-o of 3.07 (190 degrees C), corresponding to a yield of 15g oligosaccharides/100g dry feedstock. The processed solids are enriched in glucan and lignin. The maximum glucan content (35%) was attained at log R-o of 3.51 (205 degrees C). Py-GC/MS confirmed the reduction of pentose-derived carbohydrates in the solid after hydrothermal treatment and an increase of syringil units in the lignin compared to the untreated biomass. These results show the potential use of this C. ladanifer residue for the production of phenolic extracts, and hemicellulosic oligosaccharides, together with the production of a cellulose- and lignin-rich solid stream.
- Energetic potential of piggery effluent by anaerobic digestion [Resumo]Publication . Eusebio, Ana; Ramalho, Luís; Carvalheiro, Florbela; Gírio, Francisco; Marques, Isabel PaulaABSTRACT: The sector of pig farming in Portugal is looking for sustainable and practical solutions to overcome existing environmental problems caused by very polluting discharges of effluents in rivers and wastewater treatment plants. The anaerobic digestion (AD) is a suitable process used to treat an organic effluent and, simultaneously, provide the agricultural and energetic valorisation of the substrate. The main objective of this work was to evaluate the energetic potential of a piggery effluent, collected in a pig farm with 9,000 animals, estimated in a volume of 900-1,170 m3 d-1. Anaerobic digestion assays were carried out in batch mode, under anaerobic and mesophilic conditions.