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A
Afonso, D, Ribeiro AFG, Araújo P, Vital J, Madeira LM.  2018.  Phenol in Mixed Acid Benzene Nitration Systems. Industrial & Engineering Chemistry Research. 57:15942-15953., Number 46 AbstractWebsite
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Agostinho, DAS, Paninho AI, Cordeiro T, Nunes AVM, Fonseca IM, Pereira C, Matias A, Ventura MG.  2020.  Properties of κ-carrageenan aerogels prepared by using different dissolution media and its application as drug delivery systems. Materials Chemistry and Physics. 253:123290. AbstractWebsite

This work reports the synthesis of kappa-carrageenan aerogels using different dissolution and crosslinking media in order to evaluate its effects on the textural properties of the matrixes and further on the drug loading and release performance. The different aerogel samples were produced through the dissolution of the biopolymer in water with addition of potassium salts as crosslinking agents and, in two different ionic liquids (ILs) derived from imidazolium ion, being further dried with supercritical CO2. The samples were characterized by Attenuated Total Reflectance-Fourier Transform Infrared Spectroscopy (ATR-FTIR), Scanning Electron Microscopy (SEM), Nitrogen Adsorption-Desorption Analysis, Thermogravimetry (TGA) and Differential Scanning Calorimetry (DSC). The synthesized samples presented surface areas similar to the carrageenan aerogels being their structure constituted mainly by meso and macropores. The absence of ionic liquid in samples was demonstrated by DSC analysis and was corroborated by the cytotoxicity assays which revealed that cellular viability in Caco-2 cells was preserved. Tetracycline was used as a model drug and loaded in two of the prepared aerogels samples. The release experiments were performed with the composites to test in vitro drug release at physiologic pH. With a higher macroporosity, the kappa-carrageenan aerogel prepared by dissolution into ionic liquid showed a higher loading capacity than the one prepared by dissolution into water and a slightly higher release rate. The matrixes were considered to present a good potential to be used as biocompatible carriers on drug controlled delivery.

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Batista, MKS, Mestre AS, Matos I, Fonseca IM, Carvalho AP.  2016.  Biodiesel production waste as promising biomass precursor of reusable activated carbons for caffeine removal. RSC Adv.. 6:45419-45427.: The Royal Society of Chemistry AbstractWebsite

Biodiesel production generates low particle size rapeseed waste (recovered from warehouse air filtration systems) that was herein explored as promising biomass precursor of chemically activated carbons. The influence of several experimental parameters on the porosity development was investigated. No benefit was observed when solution impregnation was made nor a significant dependence of the biomass : K2CO3 ratio was observed and{,} as expected{,} high porosity development was obtained only for treatments at 700 [degree]C. Microporous materials with apparent surface area around 1000 m2 g-1 were obtained comparing favorably with literature data regarding activated carbons from rapeseed processing by-products. A selected lab-made sample and two commercial carbons were tested as adsorbents of caffeine from aqueous solution. Although commercial materials present a quicker adsorption rate{,} regarding adsorption capacity the lab-made sample reaches the same value attained by a benchmark material. The regeneration tests made over the rapeseed derived carbon through heat treatments at 600 [degree]C for 1 hour under N2 flow proved that at least two exhaustion-regeneration cycles can be made since the material retains a caffeine adsorption capacity similar to that of the fresh carbon. Therefore{,} a waste management problem of biodiesel industry - rapeseed residue - can be transformed in a valuable material with promising properties for environmental remediation processes.

Bernardo, M, Correa CR, Ringelspacher Y, Becker GC, Lapa N, Fonseca I, Esteves IAAC, Kruse A.  2020.  Porous carbons derived from hydrothermally treated biogas digestate. Waste Management. 105:170-179. AbstractWebsite

Porous carbons from digestate-derived hydrochar were produced, characterized and their performance to reclaim phosphate from water was evaluated as a preliminary approach to demonstrate their practical application. In a first step, the digestate was converted into hydrochars through hydrothermal carbonization by using two different pH conditions: 8.3 (native conditions) and 3.0 (addition of H2SO4). The resulting hydrochars did not present significant differences. Consecutively, the hydrochars were activated with KOH to produce activated carbons with enhanced textural properties. The resulting porous carbons presented marked differences: the AC native presented a lower ash content (20.3 wt%) and a higher surface area (SBET = 1106 m2/g) when compared with the AC-H2SO4 (ash content = 43.7 wt% SBET = 503 m2/g). Phosphorus, as phosphate, is a resource present in significative amount in wastewater, causing serious problems of eutrophication. Therefore, the performance of the porous carbons samples to recover phosphate – P(PO43−) – from water was evaluated through exploitation assays that included kinetic studies. The lumped model presented a good fitting to the kinetic data and the obtained uptake capacities were the same for both carbons, 12 mg P(PO43−)/g carbon. Despite the poorer textural properties of AC-H2SO4, this carbon was richer in Ca, Al, Fe, K, and Mg cations which promoted the formation of mineral complexes with phosphate anions. The results obtained in this work are promising for the future development of P(PO43−) enriched carbons that can be used thereafter as biofertilizers in soil amendment applications.

Bernardo, MMS, Madeira CAC, dos Santos Nunes NCL, Dias DACM, Godinho DMB, de Jesus Pinto MF, do Nascimento Matos IAM, Carvalho APB, de Figueiredo Ligeiro Fonseca IM.  2017.  Study of the removal mechanism of aquatic emergent pollutants by new bio-based chars, Oct. Environmental Science and Pollution Research. 24:22698–22708., Number 28 AbstractWebsite

This work is dedicated to study the potential application of char byproducts obtained in the gasification of rice husk (RG char) and rice husk blended with corn cob (RCG char) as removal agents of two emergent aquatic contaminants: tetracycline and caffeine. The chars presented high ash contents (59.5–81.5{%}), being their mineral content mainly composed of silicon (as silica) and potassium. The samples presented a strong basic character, which was related to its higher mineral oxides content. RCG char presented better textural properties with a higher apparent surface area (144 m2 g−1) and higher micropore content (V micro = 0.05 cm3 g−1). The alkaline character of both chars promoted high ecotoxicity levels on their aqueous eluates; however, the ecotoxic behaviour was eliminated after pH correction. Adsorption experiments showed that RG char presented higher uptake capacity for both tetracycline (12.9 mg g−1) and caffeine (8.0 mg g−1), indicating that textural properties did not play a major role in the adsorption process. For tetracycline, the underlying adsorption mechanism was complexation or ion exchange reactions with the mineral elements of chars. The higher affinity of RG char to caffeine was associated with the higher alkaline character presented by this char.

Bernardo, M, Rodrigues S, Lapa N, Matos I, Lemos F, Batista MKS, Carvalho AP, Fonseca I.  2016.  High efficacy on diclofenac removal by activated carbon produced from potato peel waste, Aug. International Journal of Environmental Science and Technology. 13:1989–2000., Number 8 AbstractWebsite

In the present study, a novel porous carbon obtained by K2CO3 activation of potato peel waste under optimized conditions was applied for the first time as liquid-phase adsorbent of sodium diclofenac in parallel with a commercial activated carbon. The biomass-activated carbon presented an apparent surface area of 866 m2 g−1 and well-developed microporous structure with a large amount of ultramicropores. The obtained carbon presented leaching and ecotoxicological properties compatible with its safe application to aqueous medium. Kinetic data of laboratory-made and commercial sample were best fitted by the pseudo-second-order model. The commercial carbon presented higher uptake of diclofenac, but the biomass carbon presented the higher adsorption rate which was associated with its higher hydrophilic nature which favoured external mass transfer. Both adsorbents presented adsorption isotherms that were best fitted by Langmuir model. The biomass carbon and the commercial carbon presented adsorption monolayer capacities of 69 and 146 mg g−1, and Langmuir constants of 0.38 and 1.02 L mg−1, respectively. The better performance of the commercial sample was related to its slightly higher micropore volume, but the most remarkable effect was the competition of water molecules in the biomass carbon.

Bianchi, C, Ferreira LM, Loureiro J, Rodrigues A, Duarte P, Baptista AC, Ferreira IM.  2016.  Vanadium Pentoxide Alloyed with Graphite for Thin-Film Thermal Sensors, Mar. Journal of Electronic Materials. 45:1987–1991., Number 3 AbstractWebsite

The thermoelectric (TE) properties of vanadium pentoxide (V2O5) alloyed with graphite (G) were studied as a function of its incorporation percentage. Variable weight percentages of graphite powder (0–50{%}) were added to V2O5 powder and their mixtures were evaporated by a thermal evaporation technique to form thin films with a thickness in the range of 30–80 nm. In the infrared wavelength region, the transmittance of the obtained films increased as the G percentage was increased, while in the visible range, it decreased with G up to 10{%}. The TE properties were improved when G was in the range of 10–30{%}, while it decreased for the other percentages: Seebeck coefficient (S) changed from 0.6 mV/K to 0.9 mV/K and was zero with a G of 50{%}; the electrical conductivity varied slightly from 5 ($Ømega$m)−1 to 0.7 ($Ømega$m)−1 while the mobility improved from 0.07 cm2/V s to 1.5 cm2/V s and the respective carrier concentration was reduced, from 1 × 1018 cm−3 to 4 × 1016 cm−3. These films were applied as temperature sensors evaluating the thermovoltage as a function of thermal gradient between two electrodes, in which one was maintained at room temperature.

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Castanheiro, JE, Vital J, Fonseca IM, Ramos AM.  2019.  Glycerol conversion into biofuel additives by acetalization with pentanal over heteropolyacids immobilized on zeolites. Catalysis Today. AbstractWebsite

Dodecamolydbophosphoric acid (HPMo) immobilized on USY zeolite was used as a catalyst for the acetalization of glycerol with pentanal at 70 °C. Catalysts were prepared with different amounts of heteropolyacid, and the most active sample was the HPMo2@Y catalyst (1.1 wt.%). The products of glycerol acetalization with pentanal were (2-butyl-1,3-dioxolan-4-yl)methanol, a five-member ring compound, and 2-butyl-1,3-dioxan-5-ol, a six-member ring compound. Good values of selectivity for the five-member ring compound (80–85%) were obtained with all materials. The reaction conditions were optimized using HPMo2@Y as a catalyst. The optimal conditions were determined to be 70 °C reaction temperature with 0.3 g catalyst and a 1:2.5 M ratio of glycerol to pentanal. The catalytic stability of HPMo2@Y was studied. The acetalization of glycerol with pentanal was performed using the same sample. High catalytic activity for HPMo2@Y was observed.

Castanheiro, JE, Fonseca IM, Ramos AM, Vital J.  2017.  Tungstophosphoric acid immobilised in SBA-15 as an efficient heterogeneous acid catalyst for the conversion of terpenes and free fatty acids. Microporous and Mesoporous Materials. 249:16-24. AbstractWebsite

Alkoxylation of α−pinene, β−pinene and limonene was performed in the presence of SBA-15-occluded tungstophosphoric acid (HPW). The HPW was immobilised in SBA-15 using the sol-gel method. The catalysts were characterised by N2 adsorption, FT-IR, Raman spectroscopy, X-Ray diffraction, ICP-AES and TEM. A series of catalysts with different heteropolyacid loadings ranging from 1.8 to 19.3 wt. % were prepared. PW4-SBA-15 (with 10.8 wt. %) exhibited the highest catalytic activity for the alkoxylation of α-pinene with ethanol. An approximately 53% selectivity to α-terpinyl ethyl ether was observed over the PW-SBA-15 catalysts. PW4-SBA-15 was also used as a catalyst for the alkoxylation of other terpenes, including β-pinene and limonene. The PW4-SBA-15 catalyst exhibited high catalytic stability for the alkoxylation of α-pinene with ethanol. PW4-SBA-15 was also used as a catalyst for the esterification of free fatty acids (i.e., palmitic, stearic and oleic acids) with ethanol. Good catalytic activity was observed for the PW4-SBA-15 catalyst with the different substrates used in the esterifications.

Castanheiro, JE, Vital J, Fonseca IM, Ramos AM.  2020.  Glycerol conversion into biofuel additives by acetalization with pentanal over heteropolyacids immobilized on zeolites. Catalysis Today. 346:76-80. AbstractWebsite

Dodecamolydbophosphoric acid (HPMo) immobilized on USY zeolite was used as a catalyst for the acetalization of glycerol with pentanal at 70 °C. Catalysts were prepared with different amounts of heteropolyacid, and the most active sample was the HPMo2@Y catalyst (1.1 wt.%). The products of glycerol acetalization with pentanal were (2-butyl-1,3-dioxolan-4-yl)methanol, a five-member ring compound, and 2-butyl-1,3-dioxan-5-ol, a six-member ring compound. Good values of selectivity for the five-member ring compound (80–85%) were obtained with all materials. The reaction conditions were optimized using HPMo2@Y as a catalyst. The optimal conditions were determined to be 70 °C reaction temperature with 0.3 g catalyst and a 1:2.5 M ratio of glycerol to pentanal. The catalytic stability of HPMo2@Y was studied. The acetalization of glycerol with pentanal was performed using the same sample. High catalytic activity for HPMo2@Y was observed.

Conceição, DS, Graça CAL, Ferreira DP, Ferraria AM, Fonseca IM, do Rego BAM, Teixeira ACSC, Ferreira VLF.  2017.  Photochemical insights of TiO2 decorated mesoporous SBA-15 materials and their influence on the photodegradation of organic contaminants. Microporous and Mesoporous Materials. 253:203-214. AbstractWebsite

Mesoporous silica, SBA-15, decorated with different amounts of TiO2 (anatase) were prepared by a sol-gel method followed by hydrothermal treatment and calcination, in the presence of a soft template, copolymer Pluronic 123. Tetraethyl orthosilicate (TEOS) was used as the SiO2 precursor and commercially available TiO2 anatase nanoparticles as the supported photocatalyst. The materials were characterized by transmission electron microscopy (TEM), energy dispersive X-ray analysis (EDS), N2 adsorption-desorption isotherms, raman spectroscopy, ground state diffuse reflectance (GSDR), laser induced luminescence (LIL) and X-ray photoelectron spectroscopy (XPS). The zeta potentials of the pure SBA-15, TiO2/SBA-15 substrate and the commercial anatase sample were monitored through a complete range of pH values. All the nanomaterials developed in this work were studied in terms of their photoactivity in the UV range and in the visible range, separately. In the first case, hydroxyl radicals (OH) were confirmed to be the key active oxidizers in the photodegradation of the pesticide amicarbazone in aqueous medium. On the other hand, in the visible range, and following a dye sensitization process via a fluorescent rhodamine-like dye, two different mechanisms could be identified for the formation of the superoxide radical anion, O2−.

Cordeiro, T, Castiñeira C, Mendes D, Florence Danède, Sotomayor J, Fonseca IM, Gomes da Silva M, Paiva A, Barreiros S, Cardoso MM, Viciosa MT, Correia NT, Dionisio M.  2017.  Stabilizing Unstable Amorphous Menthol through Inclusion in Mesoporous Silica Hosts. Molecular Pharmaceutics. 14:3164-3177., Number 9 AbstractWebsite
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Cordeiro, T, Santos AFM, Nunes G, Cunha G, Sotomayor JC, Fonseca IM, Florence Danède, Dias CJ, Cardoso MM, Correia NT, Viciosa TM, Dionísio M.  2016.  Accessing the Physical State and Molecular Mobility of Naproxen Confined to Nanoporous Silica Matrixes. The Journal of Physical Chemistry C. 120:14390-14401., Number 26 AbstractWebsite

The pharmaceutical drug naproxen was loaded in three different silica hosts with pore diameters of 2.4 (MCM), 3.2 (MCM), and 5.9 nm (SBA), respectively: napMCM\_2.4 nm, napMCM\_3.2 nm, and napSBA\_5.9 nm. To access the guest physical state in the prepared composites, differential scanning calorimetry (DSC), X-ray diffraction (XRD), and attenuated total reflectance Fourier transform infrared spectroscopy were used. The different techniques provided complementary information on a molecular population that was revealed to be distributed among different environments, namely the pore core, the inner pore wall, and the outer surface. It was found that naproxen is semicrystalline in the higher pore size matrix being able to crystallize inside pores; after melting it undergoes full amorphization. In the case of the lower pore size matrix, naproxen crystallizes outside pores due to an excess of filling while most of the remaining fraction is incorporated inside the pores as amorphous. Crystallinity in these two composites was observed by the emergence of the Bragg peaks in the XRD analysis, whereas for napMCM\_3.2 nm only the amorphous halo was detected. The latter only exhibits the step due to the glass transition by DSC remaining stable as amorphous at least for 12 months. The glass transition in the three composites is abnormally broad, shifting to higher temperatures as the pore size decreases, coherent with the slowing down of molecular mobility as probed by dielectric relaxation spectroscopy. For napSBA\_5.9 nm the dielectric response was deconvoluted in two processes: a hindered surface (S-) process due to molecules interacting with the inner pore wall and a faster α-relaxation associated with the dynamic glass transition due to molecules relaxing in the pore core, which seems a manifestation of true confinement effects. The drug incorporation inside a nanoporous matrix, mainly in 3.2 nm pores, was revealed to be a suitable strategy to stabilize the highly crystallizable drug naproxen in the amorphous/supercooled state and to control its release from the silica matrix, allowing full delivery after 90 min in basic media.

Cordeiro, T, Paninho AB, Bernardo M, Matos I, Pereira CV, Serra AT, Matias A, Ventura MG.  2020.  Biocompatible locust bean gum as mesoporous carriers for naproxen delivery. Materials Chemistry and Physics. 239:121973. AbstractWebsite

The work reports the impregnation of naproxen into locust bean gum mesoporous matrixes with different textural properties. The matrixes were prepared through the dissolution of the biopolymer in water and in two ionic liquids (ILs): [bmim][Cl] and [C2OHmim][Cl] and dried with scCO2. The poor water-soluble pharmaceutical drug naproxen was loaded into the matrixes and the composites were characterized by attenuated total reflectance-Fourier transform infrared spectroscopy and by differential scanning calorimetry; the results were compared with neat ILs and drug. The naproxen release from the matrixes was attempted at pH 7.4. Sustained release of naproxen in the different composites occurs, and consequently the naproxen release has lower rates compared with neat crystalline naproxen dissolution. Nevertheless, it was possible to observe small differences on release profiles for the studied composites. The higher release rate was observed for the composite where [bmim][Cl] was used as solvent, for which the calorimetric analysis revealed full amorphization of the incorporated drug. Cytotoxicity assays reveal that cellular viability in Caco-2 cells is preserved. This fact allied with the biocompatibility of locust bean gum allow for the composites potential application as naproxen controlled/sustained delivery systems with higher drug bioavailability achieved through naproxen amorphization.

Correa, CR, Bernardo M, Ribeiro RPPL, Esteves IAAC, Kruse A.  2017.  Evaluation of hydrothermal carbonization as a preliminary step for the production of functional materials from biogas digestate. Journal of Analytical and Applied Pyrolysis. 124:461-474. AbstractWebsite

Digestate from a biogas plant that uses solely biomass for biogas production was used as precursor material for the production of activated carbon as an alternative to increase its added value. The digestate was converted into hydrochar by hydrothermal carbonization varying the temperature (190–250°C), residence time (3 and 6h), and pH (5 and 7). Temperature followed by residence time had the strongest influence on the chemical composition and thermal stability of the hydrochars. A significant effect of the pH was not observed. The hydrochars were chemically activated to enhance the surface area and use them as activated carbon. As a consequence, the surface areas increased from 8 to 14m2/g (hydrochars) to 930–1351m2/g (activated carbons). Furthermore, large micropore volumes were measured (0.35–0.50cm3/g). The activated carbons were studied as adsorbents in gas phase applications, showing that the product of digestate is a very effective adsorbent for carbon dioxide (CO2). Especially the activated carbon obtained from the hydrochar produced at 250°C for 6h, which adsorbed 8.80mol CO2/kg at 30°C and 14.8bar. Additionally, the activated carbons showed a stronger affinity towards CO2 compared to methane (CH4), which makes this material suitable for the upgrading of raw biogas to biomethane.

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Dias, D, Lapa N, Bernardo M, Ribeiro W, Matos I, Fonseca I, Pinto F.  2018.  Cr(III) removal from synthetic and industrial wastewaters by using co-gasification chars of rice waste streams. Bioresource Technology. 266:139-150. AbstractWebsite

Blends of rice waste streams were submitted to co-gasification assays. The resulting chars (G1C and G2C) were characterized and used in Cr(III) removal assays from a synthetic solution. A Commercial Activated Carbon (CAC) was used for comparison purposes. The chars were non-porous materials mainly composed by ashes (68.3–92.6% w/w). The influences of adsorbent loading (solid/liquid ratio – S/L) and initial pH in Cr(III) removal were tested. G2C at a S/L of 5 mg L−1 and an initial pH of 4.50 presented an uptake capacity significantly higher than CAC (7.29 and 2.59 mg g−1, respectively). G2C was used in Cr(III) removal assays from an industrial wastewater with Cr(III) concentrations of 50, 100 and 200 mg L−1. Cr(III) removal by precipitation (uptake capacity ranging from 11.1 to 14.9 mg g−1) was more effective in G2C, while adsorption (uptake capacity of 16.1 mg g−1) was the main removal mechanism in CAC.

Dias, D, Bernardo M, Lapa N, Pinto F, Matos I, Fonseca I.  2018.  Activated carbons from the Co-pyrolysis of rice wastes for Cr(III) removal. Chemical Engineering Transactions. 65:601-606.
Dias, D, Bernardo M, Matos I, Fonseca I, Pinto F, Lapa N.  2020.  Activation of co-pyrolysis chars from rice wastes to improve the removal of Cr3+ from simulated and real industrial wastewaters. Journal of Cleaner Production. 267:121993. AbstractWebsite

Chromium is one of the most important raw materials for the European Union. Adsorption has become an important process for the recovery of metals from wastewaters, which has led to a demand for low-cost and eco-friendly adsorbents. The objective of this work was to use new and renewable carbon-based adsorbents from rice wastes in the removal/recovery of Cr(III) from synthetic and real wastewaters. Rice wastes were submitted to co-pyrolysis and the resulting char was optimized through physical and/or chemical activations/treatments. A commercial activated carbon was used for comparison purposes. All adsorbents were characterized (including an ecotoxicity test for the char precursor) and submitted to Cr(III) removal assays from a synthetic solution, in which two solid/liquid ratios (S/L) were tested (5 and 10 g/L). The CO2 activated carbon at a S/L = 5 g/L was the biomass-derived adsorbent that performed better, obtaining a maximum Cr(III) uptake capacity of 9.23 mg/g comparable to the one obtained by the commercial adsorbent at the same S/L (9.80 mg/g). The good results on this biomass-derived carbon were due to the effective volatile matter removal during the activation (from 22.7 to 4.25% w/w), which increased both surface area (from <5.0 to 325 m2/g) and ash content (from 30.0 to 40.4% w/w), allowing an increase in Cr(III) removal due to ion exchange mechanism and porosity development. The best adsorbent, under optimized conditions, was also applied to a chromium rich industrial wastewater. The results obtained in this real case application demonstrated a competition effect due to the presence of other ions.

Dias, D, Lapa N, Bernardo M, Godinho D, Fonseca I, Miranda M, Pinto F, Lemos F.  2017.  Properties of chars from the gasification and pyrolysis of rice waste streams towards their valorisation as adsorbent materials. Waste Management. 65:186-194. AbstractWebsite

Rice straw (RS), rice husk (RH) and polyethylene (PE) were blended and submitted to gasification and pyrolysis processes. The chars obtained were submitted to textural, chemical, and ecotoxic characterisations, towards their possible valorisation. Gasification chars were mainly composed of ashes (73.4–89.8wt%), while pyrolysis chars were mainly composed of carbon (53.0–57.6wt%). Silicon (Si) was the major mineral element in all chars followed by alkaline and alkaline-earth metal species (AAEMs). In the pyrolysis chars, titanium (Ti) was also a major element, as the feedstock blends contained high fractions of PE which was the main source of Ti. Gasification chars showed higher surface areas (26.9–62.9m2g−1) and some microporosity, attributed to porous silica. On the contrary, pyrolysis chars did not present a porous matrix, mainly due to their high volatile matter content. The gasification bed char produced with 100% RH, at 850°C, with O2 as gasification agent, was selected for further characterization. This char presented the higher potential to be valorised as adsorbent material (higher surface area, higher content of metal cations with exchangeable capacity, and lowest concentrations of toxic heavy metals). The char was submitted to an aqueous leaching test to assess the mobility of chemical species and the ecotoxic level for V. fischeri. It was observed that metallic elements were significantly retained in the char, which was attributed mainly to its alkaline character. This alkaline condition promoted some ecotoxicity level on the char eluate that was eliminated after the pH correction.

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Faria, P, Duarte P, Barbosa D, Ferreira I.  2017.  New composite of natural hydraulic lime mortar with graphene oxide. Construction and Building Materials. 156:1150-1157. AbstractWebsite

Recent studies show the incorporation of graphene oxide (GO) in cement composites. But these composites are frequently incompatible with original materials for building rehabilitation. To overcome this limitation, natural hydraulic lime mortars were used as matrix, and the influence of GO percentage and type of mixing was investigated. The influence on the microstructure, mechanical and physical properties was assessed. The best results were obtained with dispersed GO at concentrations of 0.05% and 0.1%. A slight improvement of mechanical and physical characteristics was achieved. This could lead to new mortars with improved properties that can be used for building rehabilitation.

Fernandes, MJ, Moreira MM, Paíga P, Dias D, Bernardo M, Carvalho M, Lapa N, Fonseca I, Morais S, Figueiredo S, Delerue-Matos C.  2019.  Evaluation of the adsorption potential of biochars prepared from forest and agri-food wastes for the removal of fluoxetine. Bioresource Technology. 292:121973. AbstractWebsite

Twelve biochars from forest and agri-food wastes (pruning of Quercus ilex, Eucalyptus grandis, Pinus pinaster, Quercus suber, Malus pumila, Prunus spinosa, Cydonia oblonga, Eriobotrya japonica, Juglans regia, Actinidia deliciosa, Citrus sinensis and Vitis vinifera) were investigated as potential low-cost and renewable adsorbents for removal of a commonly used pharmaceutical, fluoxetine. Preliminary adsorption experiments allowed to select the most promising adsorbents, Quercus ilex, Cydonia oblonga, Eucalyptus, Juglans regia and Vitis vinifera pruning material. They were characterized by proximate, elemental and mineral analysis, thermogravimetric analysis, Fourier transform infrared spectroscopy, determination of specific surface area and pH at the point of zero charge. Batch and equilibrium studies were performed, and the influence of pH was evaluated. The equilibrium was reached in less than 15 min in all systems. The maximum adsorption capacity obtained was 6.41 mg/g for the Eucalyptus biochar, which also demonstrated a good behavior in continuous mode (packed column).

Ferreira, RC, Dias D, Fonseca I, Bernardo M, Pimenta JLCW, Lapa N, de Barros MASD.  2020.  Multi-component adsorption study by using bone char: modelling and removal mechanisms. Environmental Technology. :1-16.: Taylor & Francis AbstractWebsite
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Figueira, J, Loureiro J, Marques J, Bianchi C, Duarte P, Ruoho M, Tittonen I, Ferreira I.  2017.  Optimization of Cuprous Oxides Thin Films to be used as Thermoelectric Touch Detectors. ACS Applied Materials & Interfaces. 9:6520-6529., Number 7 AbstractWebsite

The electronic and optical properties of p-type copper oxides (CO) strongly depend on the production technique as it influences the obtained phases: cuprous oxide (Cu2O) or cupric oxide (CuO), the most common ones. Cu films deposited by thermal evaporation have been annealed in air atmosphere, with temperature between 225 and 375 °C and time between 1 and 4 h. The resultant CO films have been studied to understand the influence of processing parameters in the thermoelectric, electrical, optical, morphological, and structural properties. Films with a Cu2O single phase are formed when annealing at 225 °C, while CuO single phase films can be obtained at 375 °C. In between, both phases are obtained in proportions that depend on the film thickness and annealing time. The positive sign of the Seebeck coefficient (S), measured at room temperature (RT), confirms the p-type behavior of both oxides, showing values up to 1.2 mV·°C–1 and conductivity up to 2.9 (Ω·m)−1. A simple detector using Cu2O have been fabricated and tested with fast finger touch events.

do Fraga, AC, Quitete CPB, Ximenes VL, Sousa-Aguiar EF, Fonseca IM, Rego AMB.  2016.  Biomass derived solid acids as effective hydrolysis catalysts. Journal of Molecular Catalysis A: Chemical. 422:248-257. AbstractWebsite

The conversion of cellulose into products with higher added value often includes a depolymerization step to obtain glucose, its fundamental unity. The depolymerization reaction is carried out via hydrolysis of the β-1,4-glycosidic bond. The search for a solid acid catalyst capable of breaking these bonds is gaining increasing prominence in the literature. In this regard, sulfonated carbons have shown promising results. This work evaluated the use of a residue from the extraction of palm oil as raw material for the production of sulfonated carbons. The raw material was carbonized and sulfonated. The obtained solid acids were tested in the hydrolysis of cellobiose, a dimer of glucose often used as a model compound for cellulose. The hydrolysis reaction is the first step in converting renewable carbon sources into chemical products and biofuels. Some aspects were investigated, as the effect of carbonization temperature on the concentration of sulfonic groups, the results showing that the content thereof reached a maximum value at 300°C. Regarding the hydrolysis of cellobiose, it has been identified that there is a relationship between the concentration of sulfonic acid groups and the activity of these catalysts. However, there is a drop in the turnover number as the amount of sulfonic acid sites increases. This was related to a preferred position sulfonation mechanism. Furthermore, sulfonated carbons showed higher activity than the commercial acid resins, indicating that this material may be a good option for the generation of solid acid catalysts.

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Godinho, D, Nogueira M, Bernardo M, Dias D, Lapa N, Fonseca I, Pinto F.  2019.  Recovery of Cr(III) by using chars from the co-gasification of agriculture and forestry wastes, Aug. Environmental Science and Pollution Research. 26:22723–22735., Number 22 AbstractWebsite

The aim of the present work was to assess the efficiency of biochars obtained from the co-gasification of blends of rice huskþinspace}+þinspace}corn cob (biochar 50CC) and rice huskþinspace}+þinspace}eucalyptus stumps (biochar 50ES), as potential renewable low-cost adsorbents for Cr(III) recovery from wastewaters. The two gasification biochars presented a weak porous structure (ABETþinspace}=þinspace}63–144 m2 g−1), but a strong alkaline character, promoted by a high content of mineral matter (59.8{%} w/w of ashes for 50CC biochar and 81.9{%} w/w for 50ES biochar). The biochars were used for Cr(III) recovery from synthetic solutions by varying the initial pH value (3, 4, and 5), liquid/solid (L/S) ratio (100–500 mL g−1), contact time (1–120 h), and initial Cr(III) concentration (10–150 mg L−1). High Cr(III) removal percentages (around 100{%}) were obtained for both biochars, due to Cr precipitation, at low L/S ratios (100 and 200 mL g−1), for the initial pH 5 and initial Cr concentration of 50 mg L−1. Under the experimental conditions in which other removal mechanisms rather than precipitation occurred, a higher removal percentage (49.9{%}) and the highest uptake capacity (6.87 mg g−1) were registered for 50CC biochar. In the equilibrium, 50ES biochar presented a Cr(III) removal percentage of 27{%} with a maximum uptake capacity of 2.58 mg g−1. The better performance on Cr(III) recovery for the biochar 50CC was attributed to its better textural properties, as well as its higher cation exchange capacity.