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- Toxicity reduction and biodegradability enhancement of cork processing wastewaters by ozonationPublication . Gomes, A.C.; Silva, Lúcia; Simões, Rogério; Canto, N.; Albuquerque, AntonioBiodegradability enhancement and detoxification of cork boiling wastewater (CBW) are required for the successful implementation of biological treatment options. We studied the possibility of achieving these goals through ozonation pre-treatment by experimenting on the effect of ozone dose and pH. The CBW used had a pH of 5.81, a chemical oxygen demand (COD) of 1,865 mg L-1, a biochemical oxygen demand (BOD5) of 498 mg L-1 and total phenol (TP) and tannin compounds concentrations of 523 and 399 mg L-1, respectively. The ozone doses ranged from 0.27 to 2.63 for the O-3(applied)/COD0 ratios with samples at natural pH and set to 3.33 and 9.96. Ozonation allowed the BOD20/COD ratio (biodegradability index) to increase from 0.37 to 0.63 and a toxicity reduction from 3.08 to 1.24 TU (Microtox). The corresponding removals obtained were 15.2-62.0%, 38.4-83.2% and 56.7-92.1% for COD, TP and colour, respectively. The best outcome of ozonation pre-treatment requires O-3(applied)/COD0 ratios over 1.5 and an acid pH. The increase of TP removals with ozone dose at acid pH led to biodegradability enhancement and CBW detoxification. However, for similar conditions the highest COD removals were obtained at alkaline pH due to the hydroxyl radicals' high oxidation ability but lack of selectivity.
- Biodegradability enhancement and detoxification of cork processing wastewater molecular size fractions by ozonePublication . Santos, Diana C.; Silva, Lúcia; Albuquerque, Antonio; Simões, Rogério; Gomes, A.C.Cork boiling wastewater pollutants were fractionated by sequential use of four ultrafiltration membranes and five fractions were obtained: four retentates (>100, 50-100, 20-50 and 10-20 kDa) and one permeate (<10 kDa); which were used to study the correlation of molecular size with biodegradability and toxicity before and after ozonation. The results show that molecular size is correlated with organic load and restrains biodegradability. The fraction with >100 kDa corresponds to 56% of the organic load and the one with <10 kDa only 8%. The biodegradability of fractions increased 182% with fractions molecular size reduction from >100 to < 10 kDa and the chemical oxygen demand (COD) was from 3436 to 386 mg L-1. For biodegradability enhancement the best outcome of ozonation was obtained with compounds having molecular size >20 kDa and range from 5% up to 175% for applied ozone doses to COD ratios between 0.15 and 0.38.
- Acid sulfite pretreatment in the enzymatic hydrolysis of Cytisus striatus: optimization strategyPublication . Vaz, Álvaro; Gomes, Tânia; Simões, RogérioEthanol production from lignocellulosic material includes three major steps: biomass pretreatment, which fragments the lignocellulosic matrix to facilitate the enzymes access to the substrate; hydrolysis, where the polysaccharides are converted into fermentable sugars (e.g. glucose and xylose); and finally, fermentation that produces ethanol or other biologically based chemicals (e.g. lactic acid, succinic acid). The aim of the present work was to study the effect of some operative variables of the pretreatment stage, namely sodium hydrogen sulfite and sulfuric acid loadings, temperature and time, on the release of sugars in the enzymatic hydrolysis of Cytisus striatus, performed applying a Novozymes® cocktail, with fixed charges and operating conditions. Wood branches were chipped and submitted to different reaction conditions, with a central composite experimental design 2^4+star, exploring the following variables: sulfuric acid charge (0-3%, on wood), sodium bisulfite charge (0-4 %, on wood), maximum temperature (150-190ºC) and time at maximum temperature (0-30 minutes). After pretreatment, the acid hydrolysates were recovered, the solid residues were mechanically disintegrated and thereafter subjected to enzymatic hydrolysis with an enzymatic cocktail from Novozymes®. Sugars and by-products released in the sulphite pretreatment and enzymatic treatment hydrolysates were analyzed by HPLC.
- Energy efficiency in low consistency refining: a study using a Valley beaterPublication . Vaz, Álvaro; Espírito-Santo, António; Araújo, Pedro; Simões, Rogério; Silvy, JacquesThe purpose of this work was to study the influence of pulp fiber suspensions refining operating variables on energy efficiency coefficient. Three chemical pulps with different average morphological characteristics were used, obtained from bleached kraft Pinus sylvestris, Eucalyptus globulus and Betula verrucosa. The final objective was to establish the chemical pulps refining efficiency parameters. Refining hydromechanics and energy consumption profiles were analyzed. Average normal and tangential forces on pulp suspension in the gap clearance, resulting rotor-stator distance and no-load and refining conditions power consumption were obtained. The refining trials took place in a laboratory Valley beater, and the manipulated variables were charge on the roll and rotor rotation speed. Global relationships for tangential stress and energy efficiencies in terms of rotation speed and rotor-stator gap were obtained. A relationship between energy efficiency and shear stress was obtained. The results have shown that in a Valley beater increased rotor-stator gaps reduce energy efficiency, concomitantly increasing apparent viscosity and reducing shear stress. No-load power was seen to increase with crowding factor, and thus with flocculation. Inversely, crowding factor and ultimately flocculation had an adverse effect on energy efficiency.
- Optimization of acid sulfite pretreatment in the enzymatic hydrolysis of Cytisus striatusPublication . Vaz, Álvaro; Gomes, Tânia; Simões, RogérioEthanol production from lignocellulosic material includes three major steps: biomass pretreatment, which fragments the lignocellulosic matrix to facilitate the enzymes access to the substrate; hydrolysis, where the polysaccharides are converted into fermentable sugars (e.g. glucose and xylose); and finally, fermentation that produces ethanol or other biologically based chemicals (e.g. lactic acid, succinic acid). The aim of the present work was to study the effect of some operative variables of the pretreatment stage, namely sodium h ydrogen sulfite and sulfuric acid loadings, temperature and time, on the release of sugars in enzymatic hydrolysis, performed applying a Novozymes® cocktail, with fixed charges and operating conditions. Cystisus striatus wood branches were chipped and submitted to different reaction conditions, with a central composite experimental design 2^4+star, exploring the following variables: sulfuric acid charge (0-3%, on wood), sodium bisulfite charge (0-4 %, on wood), maximum temperature (150-190ºC) and time at maximum temperature (0-30 minutes). After pretreatment, the acid hydrolysates were recovered and the solid residues were mechanically disintegrated and thereafter subjected to enzymatic hydrolysis with an enzymatic cocktail from Novozymes®. Sugars and by-products released in the sulfite pretreatment and enzymatic treatment hydrolysates were analyzed by HPLC. The percentage of material released in the acid hydrolysates was between 7 and 29.1%. Temperature and sulfuric acid load were the most important tested variables. The inhibition products represented less than 0.9% of the initial wood mass, even for the most severe reaction conditions. Enzymatic hydrolysis of polysaccharides on solid residues resulted in conversions from 6.0 to 68.9%, depending on the reaction conditions used in biomass pretreatment with sulfite and sulfuric acid. The rate of sugars release proved to be high at the beginning, gradually decreasing with contact time. The experimental data analysis using Statgraphics®Plus5 enabled us to obtain correlation expressions and conclude that all study variables influence this phase of the process, mainly temperature and sulfuric acid load. For a given sulfite load, more acidic conditions led to higher sugar release and greater fragmentation of the material, but also higher production of degradation products; moderate sodium bisulfite (1%) and sulfuric acid (2.25%) loads released practically all hemicelluloses in the raw material.
- Enzymatic hydrolysis of Cytisus striatus: acid sulfite pretreatment optimizationPublication . Vaz, Álvaro; Gomes, Tânia; Simões, RogérioEthanol production from lignocellulosic material includes three major steps: biomass pretreatment, which fragments the lignocellulosic matrix to facilitate the enzymes access to the substrate; hydrolysis, where the polysaccharides are converted into fermentable sugars (e.g. glucose and xylose) [1]; and finally, fermentation that produces ethanol or other biologically based chemicals (e.g. lactic acid, succinic acid) [2]. The aim was to study the effect of pretreatment operative variables, namely sodium bisulfite and sulfuric acid loadings, temperature and time, on released sugars in Cytisus striatus enzymatic hydrolysis with a Novozymes® cocktail. Pre-treatment intends lignin and hemicelluloses removal, reduced cellulose crystallinity and lignocellulosic network porosity increase in order to facilitate enzyme access.
- Investigation of lab-scale horizontal subsurface flow constructed wetlands treating industrial cork boiling wastewaterPublication . Gomes, Arlindo; Silva, Lúcia; Albuquerque, Antonio; Simões, Rogério; Stefanakis, AlexandrosThe feasibility and treatment efficiency of horizontal subsurface flow constructed wetlands (HSFCW) was assessed for the first time for cork boiling wastewater (CBW) through laboratory experiments. CBW is known for its high content of phenolic compounds, complex composition of biorecalcitrant and toxic nature. Two lab-scale units, one planted with Phragmites australis (CWP) and one unplanted (CWC), were used to evaluate the removals of COD, BOD, total phenolic compounds (TPh) and decolourization over a 2.5-years monitoring period under Mediterranean climatic conditions. Seven organic and hydraulic loading rates ranging from 2.6 to 11.5 g COD/m2/d and 5.7e9.1 L/m2/d were tested under average hydraulic retention time (HRT) of 5 ± 1 days required due to the CWB limited biodegradability (i.e., BOD5/ COD of 0.19). Average removals of the CWP exceeded those of the CWC and reached 74.6%, 91.7% and 69.1% for COD, BOD5 and TPh, respectively, with respective mass removals rates up to 7.0, 1.7 and 0.5 (in g/m2/d). Decolourization was limited to 35%, since it mainly depends on physical processes rather than biodegradation. CBW concentration of nine phenolic compounds ranged from 1.2 to 38.4 mg/L (for the syringic and ellagic acids, respectively) in the raw CBW, with respective removals in the CWP unit ranging from 41.8 to 76.3%, higher than those in the control unit. Despite CBWhigh concentration of TPhs (average of 116.3 mg/L), the HSFCW reached organic load removals higher than those of conventional biological treatment methods.
- Refining rheological response of chemical pulp fibre suspensionsPublication . Vaz, Álvaro; Simões, Rogério; Silvy, JacquesThe purpose of this work was to study the influence of the refining operating variables on the rheological response of chemical pulp fibre suspensions using a Valley beater. Pinus sylvestris, Eucalyptus globulus and Betula verrucosa bleached pulps were used. The normal and tangential average forces exerted on the pulp suspension in the gap clearance were evaluated, the gap between rotor and stator was measured and the apparent viscosity evolution during refining was obtained. The refining essays took place in a laboratory Valley beater, and the studied variables were the load on the roll, the rotor speed of rotation and the specific applied energy. Relationships between apparent viscosity and shear rate were tested for the three species fibre suspensions, which showed shear-thinning behaviour (Fig.1). The results were analysed in terms of fiber and flock properties. The computed crowding factors, Nc, (Kerekes and Schell) decrease from pine to eucalypt to birch. Thus, flock dimensions and resistance are significantly higher for pine. Pine had significantly wider gap, due to its greater and more resistant flocks. This produced smaller shear rate and thus higher apparent viscosity. The smaller and weaker eucalyptus and birch flocks induced smaller gaps, higher shear rates and smaller apparent viscosity. For each pulp suspension, the apparent viscosity diminished with refining time due to increased fibre flexibility and shortening, which promoted smaller flocks and reduced gap clearance (producing higher shear rates). The different rheological behaviors under the same operating conditions for different pulps lead to the inference that from the hydrodynamical point of view one should treat pulps with different morphological characteristics separately, considering the optimization of the energy transfer efficiency in pulp refining.
- Nanofibrillated cellulose rheology: effects of morphology, ethanol/acetone addition, and high NaCl concentrationPublication . Costa, Vera L.D.; Costa, Ana P.; Simões, Rogério
- Cork Boiling Wastewater Treatment in Pilot Constructed WetlandsPublication . Gomes, A.C.; Stefanakis, Alexandros; Albuquerque, António; Simões, Rogériomost studies published on the topic of cork boiling wastewater (CBW) treatment or valorization used physico-chemical treatment options rather than biological processes. However, the related costs are high and above those of the biological treatment alternative for wastewaters with similar organic loads but from different sources. Thus, con- structed wetland systems (CWs) can be an alternative to conventional biological treatment systems, namely to activated sludge systems, with the prominent virtues of low construction and operation costs. Until today, there is no study or research published for the treatment of CBW using CW systems. Thus, this investigation is a novelty and included the monitoring over a period of four years of the operation of a horizontal subsurface flow constructed wetland (HSF CW) microcosm-scale system planted with common reeds (Phragmites australis) and filled with light expanded clay aggregates (LECA), as support media for the plants and for biofilm development. The contribution of plants to the treatment was assessed by the comparison with an identical wetland unit without plantation (control bed). After this extended period of operation intended to maximize biomass development and acclimatization, which included stepwise increase of the organic load rate (OLR) up to 8.9 g COD/m2/d, the assessment of the treatment capacity of the system was done by doubling the OLR to 16.4 g COD/m2/d during 200 days.