Unidade de Investigação – LSRE-LCM – Laboratório de Processos de Separação e Reação – Laboratório de Catálise e Materiais – Polo IPLeiria
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O polo do LSRE-LCM – Laboratório de Processos de Separação e Reação – Laboratório de Catálise e Materiais do Politécnico de Leiria foi criado em 2011 e atualmente integra o maior Laboratório Associado Português em Engenharia Química, ALiCE, com uma intervenção muito relevante nas áreas de Engenharia do Ambiente e da Bioengenharia.
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- Adsorption Behavior and Mechanism of Oxytetracycline on Rice Husk Ash: Kinetics, Equilibrium, and Thermodynamics of the ProcessPublication . Andrade, Christhel A.; Zambrano-Intriago, Luis Angel; Oliveira, Nelson S.; Vieira, Judite S.; Quiroz-Fernández, Luis Santiago; Rodríguez-Díaz, Joan ManuelThe main objective of the present study is to determine the kinetics, thermodynamics, and adsorption mechanism of the oxytetracycline (OTC) on rice husk ash (RHA). The adsorbent was characterized by scanning electronic microscopy, Fourier transform infrared spectroscopy, and nitrogen physisorption. Batch studies were carried out to evaluate the influence of the adsorbent dose, initial concentration, contact time, temperature, and initial pH. RHA was characterized as having heterogeneous, fibrous, and porous particles, consisting predominantly of silica. The removal of OTC depends on the pH of the medium, which is favored at acid pH values. The kinetic data followed the Bangham model, which indicated an OTC diffusion in the pores of RHA, although this was not the only process, as demonstrated through the use of the Weber-Morris model (IPD model). The Sips isotherm best represents the experimental results of the equilibrium study. It was found that the adsorption process was spontaneous and endothermic. The highest adsorption capacity was found at a pH in the range of 4–6, when the OTC is in its zwitterion form and the surface of the RHA is positively charged, thus permitting electrostatic interactions and the formation of hydrogen bonds between the adsorbent and adsorbate molecules. These findings demonstrate the potential of rice husk ash to remove oxytetracycline from water.
- Anaerobic Mesophilic Co-Digestion of Swine Slurry and Hidrolyzate in Batch Reactors: A Case StudyPublication . Domingues, Paulo S.; Pala, Helena; Oliveira, Nelson S.The management of residual flows from swine farms, such as slurry and hydrolyzate, is a serious environmental problem in Portugal, so the search for new solutions is important, especially if they can be implemented in production sites, avoiding the transport of waste. Anaerobic co-digestion can configure a sustainable method of management and valorization of these flows in swine farms, resulting in biogas to produce energy and a digestate with agronomic value. The swine hydrolyzate is the product from the elimination of swine carcasses on the farms, through a hydrolysis process. Its use in the anaerobic process wasn’t found in the literature, identifying the need to evaluate its potential. Thus, anaerobic co-digestion of swine slurry and hydrolyzate was carried out and the main purpose of this research was to find the best feeding ratio between the two substrates in batch test, focusing on biogas production. The study was developed in two phases, both under mesophilic conditions. In the first one, using 100 ml syringes, the effect of the relative proportion of substrates on the anaerobic co-digestion potential was investigated and the effect of pressure sterilization of the substrates on biogas production was verified. In the second phase, a larger scale study was carried out in a 4,500 ml digestor, ran under the conditions identified as the most favorable in the preliminary tests. The results obtained allowed us to conclude that the largest volume of accumulated biogas was obtained with the proportion of 90.9% swine slurry: 9.1% swine hydrolyzate (v/v); and that the sterilization of the substrates doesn’t constitute an effective thermal pre-treatment. The larger scale test revealed an inefficient anaerobic process due to the inhibitory effect caused by the accumulation of ammonia and volatile organic acids. However, the production yield was 606.8 LBiogas/kgVS and 431.6 LMethane/kgVS, indicating that process allowed a production of biogas and methane higher than the values cited in literature for anaerobic digestion of swine slurry. This result showed that the use of swine hydrolyzate as a co-substrate results in a better balance of nutrients, promoting a better development of microorganisms.
- A Combined Vermifiltration-Hydroponic System for Swine Wastewater TreatmentPublication . Ispolnov, Kirill; Aires, Luis M. I.; Lourenço, Nídia D.; Vieira, Judite S.Intensive swine farming causes strong local environmental impacts by generating effluents rich in solids, organic matter, nitrogen, phosphorus, and pathogenic bacteria. Insufficient treatment of hog farm effluents has been reported for common technologies, and vermifiltration is considered a promising treatment alternative that, however, requires additional processes to remove nitrate and phosphorus. This work aimed to study the use of vermifiltration with a downstream hydroponic culture to treat hog farm effluents. A treatment system comprising a vermifilter and a downstream deep-water culture hydroponic unit was built. The treated effluent was reused to dilute raw wastewater. Electrical conductivity, pH, and changes in BOD5, ammonia, nitrite, nitrate, phosphorus, and coliform bacteria were assessed. Plants were monitored throughout the experiment. Electrical conductivity increased due to vermifiltration; pH stayed within a neutral to mild alkaline range. Vermifiltration removed 83% of BOD5, 99% of ammonia and nitrite, and increased nitrate by 11%. Hydroponic treatment removed BOD5 (63%), ammonia (100%), nitrite (66%), nitrate (27%), and phosphorus (47% total and 44% dissolved) from vermifiltered water. Coliforms were reduced by vermifiltration but recovered in the hydroponic unit. Plants showed the ability to grow on vermi-filtered wastewater, although requiring nutrient supplementation. Vermifiltration combined with hydroponics is a promising treatment for swine wastewater, although optimization will be needed for a sustainable real-scale implementation.
- Complexation and DFT studies of lanthanide ions by (2-pyridylmethoxy)homooxacalixarene derivativesPublication . Marcos, Paula M.; Teixeira, Filipa A.; Segurado, Manuel A.P.; Ascenso, José R.; Bernardino, Raul; Cragg, Peter J.; Michel, Sylvia; Hubscher-Bruder, Véronique; Arnaud-Neu, FrançoiseThe binding of lanthanide cations by 2-pyridylmethoxy derivatives of p-tert-butyldihomooxacalix[4]arene (1b), in the cone conformation, and p-tert-butylhexahomotrioxacalix[3]arene (2b), in both cone and partial cone conformations, was studied. These properties were assessed by extraction studies of the metal picrates from water into dichloromethane and stability constant measurements in methanol and acetonitrile, using spectrophotometric and microcalorimetric techniques. Proton NMR titrations with La3+ and Yb3+ cations were done in order to get information on the binding sites. Computational methods (density functional theory (DFT) calculations) were also used to complement the NMR data. The p-tert-butylcalix[4]arene analogue (3b) was also studied, and the results of the four ligands were compared. Partial cone-2b is the best extractant for lanthanide ions, showing some preference for the heavy lanthanides. In complexation, all four ligands show the same trend and a high selectivity for Yb3+ (ML, log β ≥ 7). Besides the formation of ML complexes, ML2 species were also obtained. In most cases, these species were corroborated by the proton NMR studies. For partial cone-2b with Pr3+ the complexation process is enthalpically driven, whereas for 3b the formation of the ML2 species with this cation is due to a favourable entropy term. DFT studies indicate that ligand 3b forms the most stable complex with La3+, followed by partial cone-2b.
- Complexation and DFT studies of lower rim hexahomotrioxacalix[3]arene derivatives bearing pyridyl groups with transition and heavy metal cations. Cone versus partial cone conformationPublication . Marcos, Paula M.; Teixeira, Filipa A.; Segurado, Manuel A. P.; Ascenso, José R.; Bernardino, Raul; Peter J. Cragg; Sylvia Michel; Véronique Hubscher-Bruder; Françoise Arnaud-NeuThe binding of representative alkali, alkaline earth, transition and heavymetal cations by 2-pyridylmethoxy derivatives (1b, in cone and partial cone conformations) of p-tert-butylhexahomotrioxacalix[3]arene was studied. Binding was assessed by extraction studies of the metal picrates from water into dichloromethane and by stability constant measurements in acetonitrile and methanol, using spectrophotometric and potentiometric techniques. Microcalorimetric studies of some selected complexes in acetonitrile were performed, as well as proton NMR titrations. Computational methods (density functional theory calculations) were also employed to complement the NMR data. The results are compared with those obtained with the dihomooxacalix[4]arene 2b and the calix[4]arene 3b derivative analogues. Partial cone-1b is the best extractant for transition and heavy metal cations. Both conformers of 1b exhibit very high stability constants for soft and intermediate cations Pb2+, Cd2+, Hg2+, Zn2+ and Ni2+, with cone-1b the strongest binder (ML, log b ≥7) and partial cone-1b the most selective. Both derivatives show a slight preference for Na+. Besides the formation of ML complexes, ML2 and M2L species were also observed. The former complexes were, in general, formed with the transition and heavy metal cations, whereas the latter were obtained with Ag+ and Hg2+ and partial cone-1b. In most cases, these species were corroborated by the proton NMR and density functional theory studies.
- Degradation of Oxytetracycline in Aqueous Solutions: Application of Homogeneous and Heterogeneous Advanced Oxidative ProcessesPublication . Giler-Molina, José Miguel; Zambrano-Intriago, Luis Angel; Quiroz-Fernández, Luis Santiago; Napoleão, Daniella Carla; Vieira, Judite dos Santos; Oliveira, Nelson Simões; Rodríguez-Díaz, Joan ManuelOxytetracycline is one of the antibiotics most frequently used in the Shrimp Industry during the control of bacterial diseases. These emerging pollutants, which appear in low concentrations, are persistent and alternative treatments and are required for their elimination. The degradation of oxytetracycline was evaluated in an aqueous solution by applying homogeneous (UV/H2O2 and photo-Fenton) and heterogeneous (UV/TiO2 /H2O2) advanced oxidative processes (AOPs). The studies were carried out using a bench reactor with short-wave ultraviolet lamps (UV-C). We quantified the extent to which the degradation of the drug had been efficient by employing highly efficient liquid chromatography (HPLC) and a PDA detector with a wavelength of 354 nm and a C18 column. The best results were obtained when applying the UV/H2O2 treatment, which attained a degradation of 97% under the initial conditions of a dose of 8 µL of H2O2 and 120 min of radiation. The pseudo-first order kinetic model proposed by Chan and Chu showed that the experimental results had an adequate fit, with values greater than R2 ≥ 0.95. Toxicity tests were applied to verify the effect of AOPs employed, when the drug was present in low concentrations. The test results demonstrated a decrease in the root growth of the species Lactuca sativa and Daucus carota.
- The Effect of a Naturally Ventilated Roof on the Thermal Behaviour of a Building under Mediterranean Summer ConditionsPublication . Ramos, João; Aires, LuisWith the increasing cost associated with energy consumption, climate change and the greater awareness of the population to issues related to energy and environmental efficiency, energy conservation in buildings has been encouraged, along with the development of several solutions based on a more sustainable construction. Building cooling is the most challenging issue in the Mediterranean climate. The roof is one of the main elements of the building’s opaque envelope, where the choice of materials and the implementation of appropriate passive technologies determine the thermal performance of a building. The present work aims to assess the impact of natural ventilation of a roof cavity on the thermal environment of a dwelling house under Mediterranean summer conditions. An experimental study was developed in a small-scale prototype of a typical dwelling house, comprising a ceramic tile roof with vented eaves and insulated sub-tile panels according to the construction solution of the Humbelino Monteiro SA company. The thermal performance of this roof solution was assessed under real climatic conditions based on continuous measurements of the air velocity inside the air gap, the temperature of the air and the surface temperature of all roof layers. Weather conditions were also monitored continuously. Connected with the heat transfer mechanisms, the obtained temperature and air velocity profiles data were analysed and discussed.
- Metal alginates for polyphenol delivery systems: Studies on crosslinking ions and easy-to-use patches for release of protective flavonoids in skinPublication . Silva, João; Vanat, Pavlo; Marques da Silva, Dorinda; Rodrigues, Joaquim Rui; Lagoa, RicardoIncorporation of bioactive natural compounds like polyphenols is an attractive approach for enhanced functionalities of biomaterials. In particular flavonoids have important pharmacological activities, and controlled release systems may be instrumental to realize the full potential of these phytochemicals. Alginate presents interesting attributes for dermal and other biomaterial applications, and studies were carried here to support the development of polyphenol-loaded alginate systems. Studies of capillary viscosity indicated that ionic medium is an effective strategy to modulate the polyelectrolyte effect and viscosity properties of alginates. On gelation, considerable differences were observed between alginate gels produced with Ca2+, Ba2+, Cu2+, Fe2+, Fe3+ and Zn2+ as crosslinkers, especially concerning shrinkage and morphological regularity. Stability assays with different polyphenols in the presence of alginate-gelling cations pointed to the choice of calcium, barium and zinc as safer crosslinkers. Alginate-based films loaded with epicatechin were prepared and the kinetics of release of the flavonoid investigated. The results with calcium, barium and zinc alginate matrices indicated that the release dynamics is dependent on film thicknesses, but also on the crosslinking metal used. On these grounds, an alginate-based system of convenient use was devised, so that flavonoids can be easily loaded at simple point-of-care conditions before dermal application. This epicatechin-loaded patch was tested on an ex-vivo skin model and demonstrated capacity to deliver therapeutically relevant concentrations on skin surface. Moreover, the flavonoid released was not modified and retained full antioxidant bioactivity. The alginate-based system proposed offers a multifunctional approach for flavonoid controllable delivery and protection of skin injured or under risk.
- Molecular Dissection of Escherichia coli CpdB: Roles of the N Domain in Catalysis and Phosphate Inhibition, and of the C Domain in Substrate Specificity and Adenosine InhibitionPublication . López-Villamizar, Iralis; Cabezas, Alicia; Pinto, Rosa María; Canales, José; Ribeiro, João Meireles; Rodrigues, Joaquim Rui; Costas, María Jesús; Cameselle, José CarlosCpdB is a 3′-nucleotidase/2′ 3′-cyclic nucleotide phosphodiesterase, active also with rea-sonable efficiency on cyclic dinucleotides like c-di-AMP (3′,5′-cyclic diadenosine monophosphate) and c-di-GMP (3′,5′-cyclic diadenosine monophosphate). These are regulators of bacterial physi-ology, but are also pathogen-associated molecular patterns recognized by STING to induce IFN-β response in infected hosts. The cpdB gene of Gram-negative and its homologs of gram-positive bacteria are virulence factors. Their protein products are extracytoplasmic enzymes (either periplas-mic or cell–wall anchored) and can hydrolyze extracellular cyclic dinucleotides, thus reducing the innate immune responses of infected hosts. This makes CpdB(-like) enzymes potential targets for novel therapeutic strategies in infectious diseases, bringing about the necessity to gain insight into the molecular bases of their catalytic behavior. We have dissected the two-domain structure of Escherichia coli CpdB to study the role of its N-terminal and C-terminal domains (CpdB_Ndom and CpdB_Cdom). The specificity, kinetics and inhibitor sensitivity of point mutants of CpdB, and truncated proteins CpdB_Ndom and CpdB_Cdom were investigated. CpdB_Ndom contains the catalytic site, is inhibited by phosphate but not by adenosine, while CpdB_Cdom is inactive but contains a substrate-binding site that determines substrate specificity and adenosine inhibition of CpdB. Among CpdB substrates, 3′-AMP, cyclic dinucleotides and linear dinucleotides are strongly dependent on the CpdB_Cdom binding site for activity, as the isolated CpdB_Ndom showed much-diminished activity on them. In contrast, 2′,3′-cyclic mononucleotides and bis-4-nitrophenylphosphate were actively hydrolyzed by CpdB_Ndom, indicating that they are rather independent of the CpdB_Cdom binding site.
- Optimization of an Indoor DWC Hydroponic Lettuce Production System to Generate a Low N and P Content WastewaterPublication . Aires, Luis M. I.; Ispolnov, Kirill; Luz, Tomás R.; Pala, Helena; Vieira, Judite S.Hydroponic production raises economic and environmental issues related to the treatment, recovery or disposal of hydroponic wastewater, which can be rich in eutrophication-related nutrients, nitrogen (N) and phosphorus (P). Little focus has been put on the influence of the growth conditions on the N and P content in hydroponic wastewater, which is of uttermost importance when it is intended to reuse the wastewater for irrigation or other purposes with reduced impact on the environment. This study aimed to optimize an indoor non-recirculating deep-water culture (DWC) hydroponic system for lettuce (Lactuca sativa L. var. crispa) production, in terms of daily light integral (DLI) and volume of nutrient solution (NS) per plant, to maximize both the biomass production and the N and P removal, allowing for the wastewater to meet the criteria established for reusing in irrigation and minimizing the eutrophication impacts. A small-scale DWC hydroponic system with a fluorescent light fixture was built to study lettuce growth indoors for 35 days after transplanting (DAT). A first experiment was conducted under 14, 20 or 23 mol m−2 d−1 DLI and with 1.5 or 2 L of NS per plant. A pronounced inner leaf tip burn was observed, regardless of the volume of NS solution used, related to the unventilated conditions under high radiation. Total biomass was similar in all treatments and N and P removal was higher than 95% and 94%, respectively, at 35 DAT. Lettuces grown in 2 L of NS per plant exhibited higher average biomass. A second experiment was performed under 8, 10 or 12 mol m−2 d−1 DLI and with 2 or 3 L of NS per plant, making it possible to achieve healthy biomass at 35 DAT with higher water and light-use efficiency when compared to the first experiment. A DLI of 10 or 12 mol m−2 d−1 with 2 L of NS per plant and a DLI of 12 mol m−2 d−1 with 3 L of NS per plant made it possible to achieve both the best total biomass production and the highest N and P removal from water. Under those conditions, hydroponic wastewater complied with N and P criteria for reuse in irrigation, showing potential to be used as an alternative resource for agriculture and to minimize negative impacts on the environment.