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- Chemical composition and study on liquefaction optimization of chestnut shellsPublication . Cruz-Lopes, Luísa; Domingos, Idalina; Ferreira, José; Esteves, BrunoChestnut shell (CS) is a by-product of some food sector companies. The aim of this study was to test the suitability of this material to be liquefied with polyalco- hols, optimizing the main liquefaction parameters in order to use the liquefied material for the production of high added value products. As the chemical composition of the fruit shell depends on the variation in the soil, cli- mate, and species, the chemical composition of CS was determined. Liquefaction was performed with 50:50 ethy- leneglycol:glycerol catalyzed by sulfuric acid. Different tests were carried out and several parameters were tested: par- ticle size, temperature 130–190°C, and time 15–120min. Chemical composition of CSs was determined. The main component found was lignin with 47.0%, which is higher than α-cellulose with around 20.5%, hemicelluloses 15.2%, and extractives in ethanol 8.8%. For the tested parameters, the best liquefaction yield was obtained at 190°C, 30 min, and a 40–60 particle size.
- Chemical Composition and Optimization of Liquefaction Parameters of Cytisus scoparius (Broom)Publication . Cruz-Lopes, Luísa; Almeida, Daniela; Dulyanska, Yuliya; Domingos, Idalina; Ferreira, José; Fragata, Anabela; Esteves, BrunoInvasive plants spread in such a way that they are threats to native species and to biodiversity. In this context, this work aims to determine possible valorizations of Scotch Broom Cytisus scoparius (L.) Link. This species harvested in the Viseu region was used in the present study. The eco-valorization of these renewable resources was made by conversion into liquid mixtures that can later be used in the manufacture of valuable products. For a better understanding of the results obtained, a chemical characterization of the Cytisus scoparius branches (CsB) was made. The ash content, extractives in dichloromethane, ethanol and water, lignin, cellulose and hemicellulose of the initial material were determined. Liquefaction was made in a reactor with different granulometry, temperatures and time. Results show that Broom is mainly composed of cellulose (36.1%), hemicelluloses (18.6%) and lignin (14.6%) with extractives mainly soluble in ethanol, followed by water and a small amount in dichloromethane. Ashes were around 0.69%, mainly composed of potassium and calcium. Generally, smaller size, higher solvent ratio, higher temperature and higher time of liquefaction lead to higher liquefaction. The highest percentage of liquefaction was 95% which is better than most of the lignocellulosic materials tested before.
- Termite resistance, chemical and mechanical characterization of paulownia tomentosa wood before and after heat treatmentPublication . Esteves, Bruno; Ferreira, Helena; Viana, Helder Filipe dos Santos; Ferreira, José; Domingos, Idalina; Cruz-Lopes, Luísa; Jones, D.; Nunes, L.The introduction of new species in forest management must be undertaken with a degree of care, to help prevent the spread of invasive species. However, new species with higher profitability are needed to increase forest products value and the resilience of rural populations. Paulownia tomentosa has an extremely fast growth. The objective and novelty of this work was to study the potential use of young Paulownia trees grown in Portugal by using heat treatment to improve its properties, thereby allowing higher value applications of the wood. The average chemical composition of untreated and heat-treated wood was determined. The extractive content was determined by successive Soxhlet extraction with dichloromethane (DCM), ethanol and water as solvents. The composition of lipophilic extracts was performed by injection in GC-MS with mass detection. Insoluble and soluble lignin, holocellulose and α-cellulose were also determined. Physical (density and water absorption and dimensional stability) and mechanical properties (bending strength and bending stiffness) and termite resistance was also determined. Results showed that extractive content increased in all solvents, lignin and α-cellulose also increased and hemicelluloses decreased. Compounds derived from the thermal degradation of lignin were found in heat-treated wood extractions. Dimensional stability improved but there was a decrease in mechanical properties. Resistance against termites was better for untreated wood than for heat-treated wood, possibly due to the thermal degradation of some toxic extractives.
- Valorization of Arbutus unedo L. Bark Through Chemical Composition Analysis, Liquefaction, and Bio-Based Foam ProductionPublication . Cruz-Lopes, Luísa; Dulyanska, Yuliya; Lopes, Rogério; Domingos, idalina; Ferreira, José; Esteves, BrunoArbutus unedo (strawberry tree) is a small Mediterranean tree capable of vigorous regrowth after disturbances like fire. Traditionally used for biomass fuel, its bark and branches hold potential for higher-value products through ecovalorization into liquid mixtures that could replace petroleum-based materials. This study aimed to explore the chemical composition of various components of Arbutus unedo and to produce a liquefied material from its internal (IB) and external bark (EB). Chemical compositions of internal and external bark were determined using TAPPI standards including ash, extractive content, lignin, and cellulose. Metal cations were analyzed by ICP. Liquefaction of bark was optimized in a PARR reactor, evaluating factors such as particle size, temperature, and time, and the best polyols were monitored by FTIR-ATR. Polyurethane foams were made with internal and external bark materials liquefied by polymerization with isocyanate, a catalyst, and water as a blowing agent. Results showed that EB has a higher extractive and lignin content, while IB contains more cellulose. Liquefaction yields were higher for IB (74%) than EB (68%), with IB yielding polyols that produced stronger and more resilient foams with higher compressive strength and modulus of elasticity. Mechanical properties of the foams were influenced by the NCO/OH ratio and catalyst levels. Overall, the internal bark demonstrated superior performance for foam production, highlighting its potential as an eco-friendly alternative to petroleum-derived materials.
- Liquefaction and chemical composition of walnut shellsPublication . Domingos, Idalina; Ferreira, José; Cruz-Lopes, Luísa; Esteves, BrunoThe cultivation of walnut (Juglans regia L.) for the exploitation of the fruit has been increasingly recognized worldwide; therefore, it is important to valorize a large amount of biomass from walnut shells (WS), where liquefaction may play an important role. This work intends to contribute to an improved understanding of the best uses for this material. The assays were made with a binary mixture of ethylene glycol and glycerol (1:1 v/v) as solvents, catalyzed by sulfuric acid. The tested parameters were as follows: particle size >0.420– 0.177mm, temperature 140–200°C, and reaction time between 15 and 60min. The initial dried material, the liquefied material, and the resulting solid residue were analyzed by FTIRATR for polyol characterization. The results showed that WS are mostly composed of lignin with 35.0% and polysaccharides, 30.0% cellulose and 24.9% hemicelluloses. High-lignin content indicated that WS might be used as a bio-fuel or adhesives. Extractives represent 10.2% with almost half (4.6%) of polar extractives. The best conditions to attain the optimal liquefaction yield were 160°C, 30min, and 0.420–0.250mm particle size, for the tested parameters. FTIR spectrum of the liquefied material is very different from the original material, and solid residue spectra seem to indicate that there is higher liquefaction of polysaccharides when compared with lignin since there is a higher absorption at 1,600 cm−1 and lower absorption at 1,040 cm−1 and that liquefied compounds are probably in smaller molecules.
- The Influence of Age on the Wood Properties of Paulownia tomentosa (Thunb.) Steud.Publication . Esteves, Bruno; Cruz-Lopes, Luísa; Viana, Helder Filipe dos Santos; Ferreira, José; Domingos, Idalina; Nunes, Leonel J. R.Forests in Portugal are highly dependent on a short number of wood species, and new species with higher profitability are needed. The Paulownia species has generated great interest due to its fast-growing and relatively good wood properties. However, environmental factors have shown that Paulownia grows differently in each case. This study intends to determine the properties of young Paulownia trees from Portuguese plantations to determine the best age to cut the trees according to their use. The chemical composition (extractives in dichloromethane, ethanol and water, lignin, α-cellulose, and hemicelluloses), heating value, elemental analysis (CHNO), inorganic elements and thermogravimetric analyses (TGA), and the most important mechanical and physical properties (density, MOE, bending strength, water absorption equilibrium, moisture content, and dimensional changes) were determined for 1-, 3-, and 5-year-old trees. The results show that, chemically, the extractives increased while hemicelluloses decreased with age, and no trend was found for lignin and α-cellulose. The physical and mechanical properties increased with age, except for the MOE and bending strength. The 5-year-old samples presented the best features for pellet production, namely, calorific power, elemental composition CHNO and sulfur, and inorganic elements.
- Calorific Power Improvement of Wood by Heat Treatment and Its Relation to Chemical CompositionPublication . Domingos, Idalina; Ayata, Umit; Ferreira, José; Cruz-Lopes, Luísa; Sen, Ali; Sahin, Sirri; Esteves, BrunoChemical composition influences the calorific power of wood, mainly due to the calorific power of structural compounds and extractives. Heat treatment changes the chemical composition of treated wood. This work studies the relationship between chemical composition and calorific power improvement by heat treatment. Samples were heat-treated by the ThermoWood process ® for 1 h and 2 h. High heating value (HHV) and chemical composition; lignin, cellulose, hemicelluloses and extractives in dichloromethane, ethanol, and water were determined. The HHV of untreated wood ranged between 18.54–19.92 MJ/kg and increased with heat treatment for all the tested species. A positive linear correlation was found between HHV and Klason lignin (R2 = 0.60). A negative trend was observed for holocellulose, cellulose, and hemicelluloses content against HHV, but with low determination coefficients for linear regression. The best adjust for polysaccharides was found for hemicelluloses content. A positive correlation could be found for dichloromethane extractives (R2 = 0.04). The same was obtained in relation to ethanol extractives with R2 = 0.20. For water and total extractives, no clear positive or negative trends could be achieved. The results showed that the HHV of wood increased with heat treatment and that this increase was mainly due to the increase in lignin content.
- Influence of Pre-Hydrolysis on the Chemical Composition of Prunus avium Cherry SeedsPublication . Cruz-Lopes, Luísa; Dulyanska, Yuliya; Domingos, Idalina; Ferreira, José; Fragata, Anabela; Guiné, Raquel; Esteves, BrunoDuring the industrial processing of sweet cherry fruits, the seeds are considered agricultural waste and must be disposed of, typically through burning. In this context, it is intended to contribute to the scientific development of the ecovalorization of by-products and to provide new strategies for their transformation into value-added products obtained from sweet cherry seeds (SCS). This work aimed to establish the chemical characterization of SCS before and after several pre-hydrolysis steps in order to allow the solubilization of hemicelluloses that can later be used for the recovery of sugars. The higher percentage of cellulose and lignin remaining in the solid phase will allow its further processing for an integral valorization of the raw material. The temperature (160 and 170 °C) and time (0 and 180 min) of pre-hydrolysis were optimized to obtain the best liquefaction. The percentage of liquefied material was determined from the solid waste obtained at the time of filtration. The best liquefaction by the hydrolysis of SCS was obtained at 170 °C and 180 min, with a yield of 26.7%. The chemical analyses of SCS throughout hydrolysis showed the solubilization of hemicelluloses with increases in the time and temperature of the reactor. α-cellulose and lignin showed an increase both with temperature and time, increasing the material’s potential for further processing in adhesives. FTIR analysis showed that there were significant changes in the spectra between the initial SCS, the solid residue, and the liquefied material. Pre-hydrolysis was proven to be an efficient process to improve the chemical composition of the material for further processing into adhesives or higher-mechanical-strength polyurethane foams