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- 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.
- A refinabilidade de pastas químicas papeleiras: um contributo para a sua avaliação utilizando o refinador ValleyPublication . Vaz, Álvaro Frederico Campos; Silvy, Jacques; Simões, Rogério Manuel dos SantosThe goal of this thesis is to set up a methodology to establish a relationship between pulp properties, namely morphological and physical, and paper properties, specifically structural, optical and strength, with the operating variables of refining and the physical and chemical properties of the raw material. The goal is to contribute to the analysis of the beatability of chemical pulps for paper production. The beatings took place in a laboratory Valley beater, and the studied variables were the charge on the roll, the rotor speed of rotation and the specific applied energy. For its feasibility, one fitted the following adaptations to the Valley: a rotor speed of rotation variation controller, a sensor to measure the distance between rotor and stator and an electrical power consumption meter. The effects for three different bleached Kraft pulps were studied, one being pine and the others Portuguese eucalyptus and birch. At the fibre level, its morphology was analysed by image analysis, such as the average fibre length and distribution, its width, coarseness, curl, kinks, fibrillation and fines proportion; the intrinsic fibre resistance was evaluated, such as its water retention value and wet flexibility. At the paper level, one measured its density, tensile strength, burst strength, tear strength, brightness, opacity and its scattering and absorption coefficients. One implemented methodologies to evaluate the relative bonded area and the bond strength in the paper structure using optical and mechanical methods. The hydromechanics of the beating was analysed for the three pulps. So the beating effects on the specific edge load was studied, the normal and tangential forces were evaluated, the pulp apparent viscosity evolution during refining was determined, the distance between rotor and stator was measured and also the energetic efficiency was quantified. One obtained relationships between the apparent viscosity and the rotor-stator gap, and another between the first one and the rate of shear. One explored the experimental results in order to develop control relationships for the pulp properties to paper production. One essayed an optimization of the refining conditions for each pulp for specific types of industrial papers, namely in terms of paper properties and the energy consumption in the Valley beater. The pulp suspension presents rheofluidificant behaviour and the apparent viscosity diminishes along the refining. The different pulps reveal different rheological behaviour, which leads to the inference that from the hydrodynamical point of view one should treat pulps with different morphological characteristics separately. The obtained adjustment equations for the different studied properties permit the comparison between the pulps and the study of the effects of the operating conditions. As expected, the pine revealed the best strength performance, the eucalyptus showed the best optical properties, and the birch showed a better mechanical performance relatively to the other hardwood. In what concerns the analysis of the operating conditions, one verified that the rotor speed of rotation has a major influence on the pulp and paper properties. One also inferred that the birch reveals an opposite behaviour comparatively to the pine and the eucalyptus, from the standpoint of the sped of rotation and the specific edge load.
- The effect of shear rate on apparent viscosity for different pulp suspensionsPublication . Vaz, Álvaro; Simões, Rogério; Silvy, JacquesThe goal of this work was to study the relationship between chemical pulps suspensions rheology and the operating variables of refining for three different paper fibres, namely Pinus sylvestris, Eucalyptus globulus and Betula verrucosa. The intention was the establishment of the best conditions for the refining of chemical pulps for paper production. In order to obtain that, the hydromechanics of the beating was analysed for the three pulps. So, the normal and tangential forces were evaluated, the distance between rotor and stator was measured and the pulp apparent viscosity evolution during refining was calculated. The refining essays took place in a laboratory Valley refiner, and the studied variables were the charge on the roll, the rotor speed of rotation and the specific applied energy. A global relationship between the apparent viscosity and the shear rate was finally obtained.
- 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.