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- Activity–acidity relationship in zeolite Y: Part 3. Application of Brönsted type equationsPublication . Costa, Carla; Lopes, Jose M.; Lemos, Francisco; Ribeiro, F. RamôaThe relation between activity and acidity in a variety of Y zeolite catalysts for the transformation of small olefins: ethene, propene, 1-butene and iso-butene, is presented. The acid site distribution of these samples was estimated by temperature-programmed desorption of ammonia, by using a numerical deconvolution technique. This information was then correlated with catalytic activity measurements using Brönsted type equations. Despite the complexity of calculations it is clear that this gas phase solid acid catalysed reactions follow simple rules, similar to the one observed in homogeneous processes.
- Effect of waste oil-cracking catalyst incorporation on durability of mortarsPublication . Costa, Carla; Ribeiro, M. Sofia; Brito, NunoThis paper presents research on transport properties and alkali-silica reaction (ASR) susceptibility of mortars containing a pozzolanic waste generated in the fluid catalytic cracking (wFCC) unit by the Portuguese oil-refinery. For this purpose, two series of mortars were prepared by partially replacing cement with 5%, 10% and 15% of wFCC catalyst. The main difference between the two series of mortars is the sand reactivity used in their composition. The results revealed that wFCC catalyst blended cement mortars exhibit an increased resistance against capillary water absorption and chloride migration, as well as a considerable inhibition effect on deleterious ASR expansion. However, under the adopted experimental conditions the incorporation of wFCC catalyst in mortars decreases their carbonation resistance.
- Activity–acidity relationship in zeolite Y: Part 1. Transformation of light olefinsPublication . Costa, Carla; Lopes, Jose M.; Lemos, Francisco; Ribeiro, F. RamôaReactions of ethene, propene, 1-butene and iso-butene over two series of catalysts, HNaY (prepared from NaY zeolite) and HNaUSY (prepared from NH4USY zeolite), were studied. The catalytic activity for the transformation of these olefins follows the expected order according to the ease of formation of the respective carbocations: ethene
- Shear-induced lamellar phase of an ionic liquid crystal at room temperaturePublication . Godinho, M. H.; Cruz, C.; Teixeira, Paulo; Ferreira, A. J.; Costa, Carla; Kulkarni, P. S.; Afonso, C. A. M.The phase behaviour of a number of N-alkylimidazolium salts was studied using polarizing optical microscopy, differential scanning calorimetry and X-ray diffraction. Two of these compounds exhibit lamellar mesophases at temperatures above 50 degrees C. In these systems, the liquid crystalline behaviour may be induced at room temperature by shear. Sheared films of these materials, observed between crossed polarisers, have a morphology that is typical of (wet) liquid foams: they partition into dark domains separated by brighter (birefringent) walls, which are approximately arcs of circle and meet at "Plateau borders" with three or more sides. Where walls meet three at a time, they do so at approximately 120 degrees angles. These patterns coarsen with time and both T1 and T2 processes have been observed, as in foams. The time evolution of domains is also consistent with von Neumann's law. We conjecture that the bright walls are regions of high concentration of defects produced by shear, and that the system is dominated by the interfacial tension between these walls and the uniform domains. The control of self-organised monodomains, as observed in these systems, is expected to play an important role in potential applications.
- Tailor-made SCC incorporating spent equilibrium catalyst from oil refineryPublication . Nunes, Sandra; Costa, CarlaThe spent equilibrium catalyst (ECat) is a waste generated by the oil-refinery industry with very high pozzolanic activity and, therefore, has a great potential as an addition in SCC. This paper describes research on the use of factorial Design of Experiments (DoE) approach to design SCC mortar mixtures incorporating ECat. As such, a central composite design was carried out to mathematically model the influence of mixture parameters and their coupled effects on deformability, viscosity, compressive strength, resistivity and ultrasonic pulse velocity. Thereafter, a numerical optimization technique was applied to the derived models to select the best mixture, which simultaneously maximizes different engineering properties and eco-efficiency, while maintaining self-compactability.
- Numerical optimization of self-compacting mortar mixture containing spent equilibrium catalyst from oil refineryPublication . Nunes, Sandra; Costa, CarlaAs the oil refining industries continue to grow, the production of waste catalysts generated in that process is expected to also increase. It would be of great value both economically and ecologically if these wastes could be reused as an addition in self-compacting concrete (SCC). This paper uses statistical factorial design approach, namely a central composite design, to conduct a proper experimental plan to design SCC mortar mixtures incorporating spent equilibrium catalyst (ECat), a waste generated by the oil refinery industry. The mathematical empirical models derived (which were also experimentally validated) revealed the influence of mixture design parameters, and their coupled effects, on the mortars' properties namely, deformability, viscosity, compressive strength, resistivity and ultrasonic pulse velocity. A numerical optimization technique was applied to the derived models to select the best mixture, which maximizes simultaneously durability and eco-efficiency and minimize cost, while maintaining self-compactability. The current study revealed that ECat can be successfully applied in SCC mortars, as a high volume cement replacement material (up to V-Ecat/Vp = 19.7%) due to its high pozzolanic activity. Nevertheless, for powder-type SCC5, cement/ECat blends must be combined with other finer additions to complete the powders distribution curve increasing the viscosity and stability of paste phase, in the fresh state.
- Hydraulic bindersPublication . Costa, CarlaHydraulic binders play a vital role in the economic and social development because they are essential components of concrete, the most widely used construction material. Nowadays, Portland cement is the most predominantly used hydraulic binder due to its properties and widespread availability. Cement manufacture consumes large amount of non-renewable raw materials and energy, and it is a carbon-intensive process. Many efforts are, therefore, being undertaken towards the developing “greener” hydraulic binders. Concomitantly, binders must also correspond to market demand in terms of performance and aesthetic as well as fulfill mandatory regulations. In order to pursue these goals, different approaches have been followed including the improvement of the cement manufacturing process, production of blended cements, and testing innovative hydraulic binders with a different chemistry. This chapter presents a brief history of hydraulic binder’s discovery and use as well as the environmental and economic context of cement industry. It, then, describes the chemistry and properties of currently most used hydraulic binders—common cements and hydraulic limes—and that of the more promising binders for future applications, namely special Portland cements, aluminous cements, calcium sulfoaluminate cements, and alkali-activated cements.
- Multi-level study on UHPFRC incorporating ECatPublication . Abrishambaf, Amin; Pimentel, Mário; Nunes, Sandra; Costa, CarlaThe suitability of a recently developed ultra-high performance fibre reinforced cementitious composite (UHPFRC) incorporating Spent Equilibrium Catalyst, ECat, for structural applications is investigated through a systematic multi-level investigation across micro, meso and composite levels. Scanning electron microscopy, isothermal calorimetry, thermogravimetric analysis, and mercury intrusion porosimetry tests were performed to evaluate the microstructure of the composite. At the meso-level, the mechanical properties of fibre to matrix ITZ were characterised by single fibre pullout tests on fibres embedded with various fibre orientation angles. At the composite level, specimens with 3% fibre content and different fibre orientation profiles were prepared to determine uniaxial tensile behaviour. The relation between the tensile fracture parameters and fibre structure parameter was assessed. In each level, the results are compared to a conventional ternary UHPFRC mixture and point towards the suitability of the newly developed mixture for structural applications.
- Feasibility of eco-friendly binary and ternary blended binders made of fly-ash and oil-refinery spent catalyst in ready-mixed concrete productionPublication . Costa, Carla; Marques, José CarlosLarge-scale recycling of new industrial wastes or by-products in concrete has become a crucial issue for construction materials sustainability, with impact in the three pillars (environmental, social and economic), while still maintaining satisfactory, or improved, concrete performance. The main goal of the paper is to evaluate the technological feasibility of the partial, or total, replacement of fly-ashes (FA), widely used in ready-mixed concrete production, with spent equilibrium catalyst (ECat) from the oil-refinery industry. Three different concrete mixtures with binary binder blends of FA (33.3% by mass, used as reference) and of ECat (16.7% and 33.3%), as well as a concrete mixture with a ternary binder blend with FA and ECat (16.7%, of each) were tested regarding their mechanical properties and durability. Generically, in comparison with commercial concrete (i) 16.7% ECat binary blended concrete revealed improved mechanical strength and durability; (ii): ternary FA-ECat blended binder concrete presented similar properties; and (iii) 33% ECat binary blended concrete has a lower performance. The engineering performance of all ECat concretes meet both the international standards and the reference durability indicators available in the scientific literature. Thus, ECat can be a constant supply for ready-mixed eco-concretes production, promoting synergetic waste recycling across industries.
- Activity–acidity relationship in zeolite ZSM-5. Application of Brönsted-type equationsPublication . Costa, Carla; Dzikh, I. P.; Lopes, Jose M.; Lemos, Francisco; Ribeiro, Fernando RamôaIn this paper the relation between activity and acidity in a variety of ZSM-5 zeolite catalysts, with different Si/Al ratios and different protonic content, is analysed and a quantitative correlation is obtained. The acid site strength distribution was estimated using temperature-programmed desorption (TPD) of ammonia by applying a digital deconvolution method to the curves. These data were then correlated with experimental catalytic activity data for the same catalysts towards n-heptane cracking reaction, by means of a Brönsted-type equation similar to the ones used for homogeneous acid catalysis and already used for other zeolites. It can be noticed that the same types of equation that are used for homogeneous acid catalysis also hold for heterogeneous acid catalysis and that the activation energy for ammonia desorption can be used as acid-strength scale for the purpose of correlation with catalytic activity.
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