The problem of brines disposal has raised great interest towards new strategies for their valorisation through the recovery of minerals or energy. As an example, the spent brine from ion exchange resins regeneration is often discharged into rivers or lakes, thus impacting on the process sustainability. However, such brines can be effectively reconcentrated, after removal of bivalent cations, and reused for the resins regeneration. This work focuses on developing and testing a pilot plant for selective recovery of magnesium and calcium from spent brines exploiting a novel proprietary crystallization unit. This is part of a larger treatment chain for the complete regeneration of the brine, developed within the EU-funded ZERO BRINE project. The pilot crystallizer was tested with the retentate of the nanofiltration unit processing the spent brine from the industrial water production plant of Evides Industriewater B.V. (Rotterdam, The Netherlands).Magnesium and calcium hydroxide were selectively precipitated by adding alkaline solution in two consecutive steps and controlling reaction pH. Performance was assessed in terms of recovery efficiency and purity of produced crystals, observing in most investigated cases a recovery of about 100% and 97% and a purity above 90% and 96%, for magnesium and calcium hydroxide, respectively.
A novel technology, the ion exchange membrane crystallizer (CrIEM), that combines reactive and membrane crystallization, was investigated in order to recover high purity magnesium hydroxide from multi-component artificial and natural solutions. In particular, in a CrIEM reactor, the presence of an anion exchange membrane (AEM), which separates two-compartment containing a saline solution and an alkaline solution, allows the passage of hydroxyl ions from the alkaline to the saline solution compartment, where crystallization of magnesium hydroxide occurs, yet avoiding a direct mixing between the solutions feeding the reactor. This enables the use of low-cost reactants (e.g., Ca(OH)2) without the risk of co-precipitation of by-products and contamination of the final crystals. An experimental campaign was carried out treating two types of feed solution, namely: (1) a waste industrial brine from the Bolesław Śmiały coal mine in Łaziska Górne (Poland) and (2) Mediterranean seawater, collected from the North Sicilian coast (Italy). The CrIEM was tested in a feed and bleed modality in order to operate in a continuous mode. The Mg2+ concentration in the feed solutions ranges from 0.7 to 3.2 g/L. Magnesium recovery efficiencies from 89 up to 100% were reached, while magnesium hydroxide purity between 94% and 98.8% was obtained.
Increasing attention is nowadays paid to the management and valorisation of industrial waste brines aiming also at the recovery of raw materials. Magnesium has been listed as a Critical Raw Material by EU, prompting researchers to investigate novel routes for its recovery. Within this framework, a novel Crystallizer with Ion Exchange Membrane (CrIEM), is proposed as an innovative way to recover magnesium from industrial waste brines exploiting low-cost alkaline reactants. In the present work, a novel mathematical model of the CrIEM process is proposed to provide a useful tool for its design in different working conditions. Batch and feed & bleed continuous configurations have been investigated taking into account: (i) the variation of the alkaline and brine concentration in their own collection tanks over time and (ii) the spatial monodimensional (1D) steady-state description of the main phenomena that occur inside the CrIEM.Original experimental data, from ad-hoc laboratory tests, and literature information were used to validate the proposed model both in the batch and continuous feed & bleed configuration. A good agreement between model predictions and experimental/literature data was found for both cases, thus proving the reliability of the proposed model for the design of the CrIEM reactor.
Three polyaminocyclodextrin materials, obtained by direct reaction between heptakis(6-deoxy-6-iodo)-β-cyclodextrin and the proper linear polyamines, were investigated for their binding properties, in order to assess their potential applications in biological systems, such as vectors for simultaneous drug and gene cellular uptake or alternatively for the protection of macromolecules. In particular, we exploited polarimetry to test their interaction with some model p-nitroaniline derivatives, chosen as probe guests. The data obtained indicate that binding inside the host cavity is mainly affected by interplay between Coulomb interactions and conformational restraints. Moreover, simultaneous interaction of the cationic polyamine pendant bush at the primary rim was positively assessed. Insights on quantitative aspects of the interaction between our materials and polyanions were investigated by studying the binding with sodium alginate. Finally, the complexation abilities of the same materials towards polynucleotides were assessed by studying their interaction with the model plasmid pUC19. Our results positively highlight the ability of our materials to exploit both the cavity and the polycationic branches, thus functioning as bimodal ligands.
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