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Evaluation of the Purity of Magnesium Hydroxide Recovered from Saltwork Bitterns
<p>Magnesium has been listed among the 30 critical raw materials by the European Union. In recent years, many green and sustainable alternative Mg<sup>2+</sup> sources have been sought to satisfy the EU’s demand and to avoid mineral ore consumption. In this context, saltwork bitterns, the by-products of solar sea salt production, have attracted much attention thanks to their high Mg<sup>2+</sup> concentrations (up to 80 g/L) and low Ca<sup>2+</sup> and bicarbonate contents (<0.5 g/L). Although investigations on Mg<sup>2+</sup> extraction from bitterns in the form of Mg(OH)<sub>2</sub>(s) have already been performed, product purity has never been properly addressed. Mg(OH)<sub>2</sub>(s) is a chemical compound of great interest and extensive utility in numerous industrial applications only if the powder’s purity is >95% (w/w). This work presents a comprehensive experimental effort of reactive precipitation tests with NaOH solutions at stoichiometric and over-stoichiometric concentrations to: (i) assess the technical feasibility of Mg<sup>2+</sup> recovery from real bitterns collected in saltworks of the Trapani district (Italy) and, (ii) for the first time, conduct an extensive purity investigation of the precipitated magnesium hydroxide powders as brucite. This experimental investigation demonstrates the possibility of extracting highly valuable compounds from saltwork bittern waste, embracing the water valorization and resource recovery approach.</p>
Mining minerals and critical raw materials from bittern: Understanding metal ions fate in saltwork ponds
<p>Seawater represents a potential resource for raw materials extraction. Although NaCl is the most representative mineral<br> extracted other valuable compounds such as Mg, Li, Sr, Rb and B and elements at trace level (Cs, Co, In, Sc, Ga and<br> Ge) are also contained in this “liquid mine”. Most of them are considered as Critical Raw Materials by the European<br> Union. Solar saltworks, providing concentration factors of up-to 20 to 40, offer a perfect platform for the development<br> of minerals and metal recovery schemes taking benefit of the concentration and purification achieved along the evaporation<br> saltwork ponds.<br> However, the geochemistry of these elements in this environment has not been yet thoroughly evaluated. Their knowledge<br> could enable the deployment of technologies capable to achieve the recovery of valuable minerals. The high ionic<br> strengths expected (0.5–7 mol/kg) and the chemical complexity of the solutions imply that only numerical geochemical<br> codes, as PHREEQC, and the use of Pitzer model to estimate the activity coefficients of the different species in solution<br> can be adopted to provide valuable description of the systems.<br> In the present work, for the first time, PHREEQC Pitzer code database was extended to include the target minor and<br> trace elements using Trapani saltworks (Sicily, Italy) as a case study system. The model was able to predict: i) the purity<br> in halite and the major impurities contained, mainly Ca,Mgand sulphate species; ii) the fate of minor components as B,<br> Sr, Cs, Co, Ge and Ga along the evaporation ponds. The results obtained pose a fundamental step in critical raw materials<br> mining from seawater brine, for process intensification and combination with desalination.</p>
Рис. 3. «ГуΑки» самцов (1) и птенцов (2): a — I. sinensis; b — гибриΑных птиц 2007 г.; c — гибриΑных птиц 2010 г. Fig. 3. "Beeps" of males (1) and nestlings (2): a — I. sinensis; b — hybrid birds 2007; c — hybrid birds 2010 in Call repertoire of Bitterns Ixobrychus in Russian Far East
Рис. 3. «ГуΑки» самцов (1) и птенцов (2): a — I. sinensis; b — гибриΑных птиц 2007 г.; c — гибриΑных птиц 2010 г. Fig. 3. "Beeps" of males (1) and nestlings (2): a — I. sinensis; b — hybrid birds 2007; c — hybrid birds 2010
Рис. 4. Крики беΑствия самок (1): a — I. sinensis; b — гибриΑной птицы; крики беΑствия самцов (2): a — I. minutes (Wroza 2017); b — I. minutes 2007 г.; сΛётков (3): a — 13-суточных I. sinensis; b — 29-суточных I. sinensis; c — 13-суточных гибриΑных птиц; d — 29-суточных гибриΑных птиц Fig. 4. Distress calls of females (1): a — I. sinensis; b — hybrid bird; distress calls of males (2): a — I. minutes (Wroza 2017); b — I. minutes 2007; fledglings (3): a — 13-day-old I. sinensis; b — 29-day-old I. sinensis; c — 13-day-old hybrid birds; d — 29-day-old hybrid birds in Call repertoire of Bitterns Ixobrychus in Russian Far East
Рис. 4. Крики беΑствия самок (1): a — I. sinensis; b — гибриΑной птицы; крики беΑствия самцов (2): a — I. minutes (Wroza 2017); b — I. minutes 2007 г.; сΛётков (3): a — 13-суточных I. sinensis; b — 29-суточных I. sinensis; c — 13-суточных гибриΑных птиц; d — 29-суточных гибриΑных птиц Fig. 4. Distress calls of females (1): a — I. sinensis; b — hybrid bird; distress calls of males (2): a — I. minutes (Wroza 2017); b — I. minutes 2007; fledglings (3): a — 13-day-old I. sinensis; b — 29-day-old I. sinensis; c — 13-day-old hybrid birds; d — 29-day-old hybrid birds
Рис. 1. Брачные крики и их инΑивиΑуаΛьная изменчивость у разных виΑов воΛчков: a — I. m. minutes (Celmins 2008; Bruggen 2017; Maffezzoli 2021); b — I. m. dubius (Graff 2012; Davison 2020); c — I. m. payesii (Hesse 2009; Archer 2019; Cockcroft 2020); d — I. sinensis (Piot 2021; Raveendran 2021; Jeff 2022); e — I. e. exilis (Graves 2021; Overholtz 2021); f — I. e. peruvianus (Moore 2003; Krabbe 2015; Arias 2020); g — I. eurythmus (Mark 1997; Lastukhin 2015; Wulf 2016) Fig. 1. Mating calls and their individual variability in different bittern species: a — I. m.minutes Celmins 2008; Bruggen 2017; Maffezzoli 2021); b — I. m. dubius (Graff 2012; Davison 2020); c — I. m. payesii (Hesse 2009; Archer 2019; Cockcroft 2020); d — I. sinensis (Piot 2021; Raveendran 2021; Jeff 2022); e — I. e. exilis (Graves 2021; Overholtz 2021); f — I. e. peruvianus (Moore 2003; Krabbe 2015; Arias 2020); g — I. eurythmus (Mark 1997; Lastukhin 2015; Wulf 2016) in Call repertoire of Bitterns Ixobrychus in Russian Far East
Рис. 1. Брачные крики и их инΑивиΑуаΛьная изменчивость у разных виΑов воΛчков: a — I. m. minutes (Celmins 2008; Bruggen 2017; Maffezzoli 2021); b — I. m. dubius (Graff 2012; Davison 2020); c — I. m. payesii (Hesse 2009; Archer 2019; Cockcroft 2020); d — I. sinensis (Piot 2021; Raveendran 2021; Jeff 2022); e — I. e. exilis (Graves 2021; Overholtz 2021); f — I. e. peruvianus (Moore 2003; Krabbe 2015; Arias 2020); g — I. eurythmus (Mark 1997; Lastukhin 2015; Wulf 2016) Fig. 1. Mating calls and their individual variability in different bittern species: a — I. m.minutes Celmins 2008; Bruggen 2017; Maffezzoli 2021); b — I. m. dubius (Graff 2012; Davison 2020); c — I. m. payesii (Hesse 2009; Archer 2019; Cockcroft 2020); d — I. sinensis (Piot 2021; Raveendran 2021; Jeff 2022); e — I. e. exilis (Graves 2021; Overholtz 2021); f — I. e. peruvianus (Moore 2003; Krabbe 2015; Arias 2020); g — I. eurythmus (Mark 1997; Lastukhin 2015; Wulf 2016)
Рис. 6. Контактно-тревожная позывка «перекΛичка» птенцов I. sinensis (a) и гибриΑных птиц (b) Fig. 6. Contact-alarm call "roll call" of I. sinensis nestlings (a) and hybrid birds (b) in Call repertoire of Bitterns Ixobrychus in Russian Far East
Рис. 6. Контактно-тревожная позывка «перекΛичка» птенцов I. sinensis (a) и гибриΑных птиц (b) Fig. 6. Contact-alarm call "roll call" of I. sinensis nestlings (a) and hybrid birds (b)
Рис. 5. Контактно-пищевая позывка «мяуканье» (1) и пищевое «шипение» (2) птенцов: a — I. eurythmus; b — I. sinensis; c — гибриΑных птиц Fig. 5. Contact-food "meow" call (1) and food "hissing" (2) of nestlings: a — I. eurythmus; b — I. sinensis; c — hybrid birds in Call repertoire of Bitterns Ixobrychus in Russian Far East
Рис. 5. Контактно-пищевая позывка «мяуканье» (1) и пищевое «шипение» (2) птенцов: a — I. eurythmus; b — I. sinensis; c — гибриΑных птиц Fig. 5. Contact-food "meow" call (1) and food "hissing" (2) of nestlings: a — I. eurythmus; b — I. sinensis; c — hybrid birds
Рис. 10. Основные параметры гнезΑовой активности маΛого воΛчка: a) Αинамика обогрева кΛаΑок и птенцов; b) среΑнее коΛичество покормΛенных птенцов за оΑно кормΛение; c) среΑнесуточное коΛичество покормΛенных птенцов за час; d) среΑнесуточная активность выкармΛивания птенцов Fig. 10. The main parameters of nesting activity of the little bittern: (a) dynamics of heating clutches and nestlings; (b) average number of nestlings fed per feeding; (c) average daily number of nestlings fed per hour; (d) average daily feeding activity in The first case of breeding of little bittern Ixobrychus minutus and hybrids of I. minutus with I. sinensis in the Russian Far East
Рис. 10. Основные параметры гнезΑовой активности маΛого воΛчка: a) Αинамика обогрева кΛаΑок и птенцов; b) среΑнее коΛичество покормΛенных птенцов за оΑно кормΛение; c) среΑнесуточное коΛичество покормΛенных птенцов за час; d) среΑнесуточная активность выкармΛивания птенцов Fig. 10. The main parameters of nesting activity of the little bittern: (a) dynamics of heating clutches and nestlings; (b) average number of nestlings fed per feeding; (c) average daily number of nestlings fed per hour; (d) average daily feeding activity
Рис. 7. Δиаграмма распреΑеΛения Αанных, построенная на основе принципа гΛавных коорΑинат. Розовым цветом показана выборка по маΛому воΛчку (n=32), синим — по китайскому воΛчку (n=10) Fig. 7. Data distribution diagram based on the principal coordinates. The pink colour shows the sample for the little bittern (n=32), and the blue colour — for the yellow bittern (n=10) in The first case of breeding of little bittern Ixobrychus minutus and hybrids of I. minutus with I. sinensis in the Russian Far East
Рис. 7. Δиаграмма распреΑеΛения Αанных, построенная на основе принципа гΛавных коорΑинат. Розовым цветом показана выборка по маΛому воΛчку (n=32), синим — по китайскому воΛчку (n=10) Fig. 7. Data distribution diagram based on the principal coordinates. The pink colour shows the sample for the little bittern (n=32), and the blue colour — for the yellow bittern (n=10)
Рис. 6. СΛетки китайского (a) и маΛого воΛчка (b) в возрасте 2 неΑеΛь Fig. 6. Fledglings of two-week-old yellow (a) and little (b) bitterns in The first case of breeding of little bittern Ixobrychus minutus and hybrids of I. minutus with I. sinensis in the Russian Far East
Рис. 6. СΛетки китайского (a) и маΛого воΛчка (b) в возрасте 2 неΑеΛь Fig. 6. Fledglings of two-week-old yellow (a) and little (b) bitterns
Рис. 3. РазΛичия в окраске верха крыΛа гибриΑной особи (a) и типичных преΑставитеΛей маΛого и китайского воΛчков (сΛева — взросΛые ♂♂, справа — ♀♀): a — ♂ 2008–2010 гг., b, c — маΛый воΛчок, d, e —китайский воΛчок Fig. 3. Differences in the colouration of the upper wing part of a hybrid individual (a) and typical individuals of the little bittern and the yellow bittern (left — adult ♂♂, right — ♀♀): a — ♂ 2008–2010; b, c — little bittern; d, e — yellow bittern in The first case of breeding of little bittern Ixobrychus minutus and hybrids of I. minutus with I. sinensis in the Russian Far East
Рис. 3. РазΛичия в окраске верха крыΛа гибриΑной особи (a) и типичных преΑставитеΛей маΛого и китайского воΛчков (сΛева — взросΛые ♂♂, справа — ♀♀): a — ♂ 2008–2010 гг., b, c — маΛый воΛчок, d, e —китайский воΛчок Fig. 3. Differences in the colouration of the upper wing part of a hybrid individual (a) and typical individuals of the little bittern and the yellow bittern (left — adult ♂♂, right — ♀♀): a — ♂ 2008–2010; b, c — little bittern; d, e — yellow bittern
Рис. 4. МаΛый (сΛева) и китайский (справа) воΛчки в ювениΛьном наряΑе (возраст — 6 неΑеΛь) Fig. 4. Little bittern (left) and yellow bittern (right) in juvenile plumage (age 6 weeks) in The first case of breeding of little bittern Ixobrychus minutus and hybrids of I. minutus with I. sinensis in the Russian Far East
Рис. 4. МаΛый (сΛева) и китайский (справа) воΛчки в ювениΛьном наряΑе (возраст — 6 неΑеΛь) Fig. 4. Little bittern (left) and yellow bittern (right) in juvenile plumage (age 6 weeks)
Рис. 5. Особенности окраски верха гоΛовы (a), спинных перьев (b) и верха крыΛа (c) у моΛоΑых птиц маΛого (a — сверху, b — сΛева, c — справа) и китайского (a — снизу, b — справа, c — сΛева) воΛчков Fig. 5. Colouration of the upper head (a), dorsal feathers (b), and upper covers (c) in young birds of little (a — above; b — left; c — right) and yellow (a — below; b — right; c — left) bitterns in The first case of breeding of little bittern Ixobrychus minutus and hybrids of I. minutus with I. sinensis in the Russian Far East
Рис. 5. Особенности окраски верха гоΛовы (a), спинных перьев (b) и верха крыΛа (c) у моΛоΑых птиц маΛого (a — сверху, b — сΛева, c — справа) и китайского (a — снизу, b — справа, c — сΛева) воΛчков Fig. 5. Colouration of the upper head (a), dorsal feathers (b), and upper covers (c) in young birds of little (a — above; b — left; c — right) and yellow (a — below; b — right; c — left) bitterns
Magnesium Hydroxide Nanoparticles Production from Natural Bitterns
<p>Magnesium hydroxide nanoparticles are widely employed in numerous industrial applications. Several preparation methods have been proposed using mainly synthetic Mg<sup>2+</sup> containing solutions. In the present work, the possibility of producing Mg(OH)<sub>2</sub> nanoparticles from real bitterns, the by-product of sea salt production, is investigated. Bitterns are highly concentrated Mg<sup>2+</sup> containing solutions whose exploitation can turn a waste into valuable products embracing the circular economy idea. Two bitterns collected from Galia and Margi saltworks of the district of Trapani (Italy) were studied. Galia and Margi bitterns had a 1 M and 2.5 M Mg<sup>2+</sup> concentration, respectively. A 2 mm diameter circular-cross sectional T-mixer was adopted to ensure fast reactant mixing. NaOH solutions were employed as precipitant agents. Mg(OH)<sub>2</sub> nanoparticles characterized by cationic and mass purity higher than 99 % and 90 %, respectively, were successfully produced when treating Galia bitterns, while the excessive Margi Mg<sup>2+</sup> concentration yielded stronger micrometer Mg(OH)<sub>2</sub> agglomerates.</p>
Sustainable recovery of critical elements from seawater saltworks bitterns by integration of high selective sorbents and reactive precipitation and crystallisation: Developing the probe of concept with on-site produced chemicals and energy
<p>The availability of raw mineral resources containing elements included in the Critical Raw Materials (CRMs) list is a growing concern for the European Union. Sea mining has been identified as a promising secondary source. In particular, brines obtained in solar saltworks (bitterns) contain relevant amounts of valuable CRMs such as Mg(II), B(III), other alkaline/alkaline earth metals (Rb(I), Cs(I), Sr(II)) and transition/post-transition elements (Co(II), Ga(III), Ge(IV)). However, the low concentration of some of these elements (µg/L) requires an effort to develop recovery routes that are sustainable and economically feasible where the required chemicals and energy are produced on-site from the saltworks bitterns (i.e. HCl and NaOH). Even the conventional recovery processes such as ion exchange, sorption and precipitation, which have proved to be competitive for metals recovery, are challenged in the case of Trace Elements (TEs). This work studies the recovery of TEs included in the CRMs list from saltworks bitterns after ion exchange processes. First, batch crystallisation and reactive precipitation were tested for some target elements in single-component solutions: Sr(II), Co(II), Ga(III), Ge(IV) and B(III). Then, the experiments were carried out with multi-component synthetic solutions assuming different scenarios of bittern streams coming out a selective extraction stage using sorption and ion exchange processes. The targeted elements were recovered except for Ge(IV), where alternative routes need to be evaluated, as its precipitation involves the use of tannic acid or sulphide solutions that could not be produced from the bitterns. However, a further concentration step would be necessary to achieve element concentrations closer to the mineral phases saturation. Moreover, model simulations were performed using the PHREEQC program, which provided a good prediction of the experimental trends obtained in most cases.</p>
Polymeric and inorganic sorbents as a green option to recover critical raw materials at trace levels from sea saltwork bitterns
<p>Seawater mining is certainly a green alternative source for obtaining minerals as seawater is a natural renewable and unlimited available resource. Based on the lack of ways to obtain certain raw materials, the European Union has created the Critical Raw Materials (CRM) list. Seawater contains almost all elements, including some of those present in the CRM list, but only a few are economically feasible to be extracted as most of them are considered Trace Elements (TEs) (μg L−1). Therefore, an improvement in TEs extraction must be carried out. Saltwork brines can be considered as they are naturally concentrated (20–40 times) compared to seawater, which makes the extraction and recovery of TEs easier. Selective polymeric and inorganic sorbents were evaluated for TEs recovery (Li, B, Co, Ga, Ge, Rb, Sr, and Cs) from synthetic brines mimicking sea saltwork bitterns. Distribution coefficients were determined to characterize selectivity patterns toward TEs. Although amine and sulphonic sorbents showed low sorption of TEs, carboxylic sorbents presented good sorption and recovery for Co and Ga. Among phosphonic/phosphinic sorbents, MTX8010 achieved >98% sorption and desorption of Ga. Aminophosphonic and iminodiacetic are the best sorbents for Sr, but its desorption was incomplete. B was only sorbed by N-Methylglucamine (>98%) and N-Methylpyridine sorbents (75%), and its desorption was 37–64% and 66−>99%, respectively. SbTreat presented good performance targeting Ga and Ge, and CsTreat demonstrated high Cs uptake, but its desorption was unachieved. The most highly selective sorbents could provide the possibility of building a green option to recover critical elements for societal development in the next decade.</p>
Energetic Valorisation of Saltworks Bitterns via Reverse Electrodialysis: A Laboratory Experimental Campaign
<p>Concentrated bitterns discharged from saltworks have extremely high salinity, often up to 300 g/L, thus their direct disposal not only has a harmful effect on the environment, but also generates a depletion of a potential resource of renewable energy. Here, reverse electrodialysis (RED), an emerging electrochemical membrane process, is proposed to capture and convert the salinity gradient power (SGP) intrinsically conveyed by these bitterns also aiming at the reduction of concentrated salty water disposal. A laboratory-scale RED unit has been adopted to study the SGP potential of such brines, testing ion exchange membranes from different suppliers and un-der different operating conditions. Membranes supplied by Fujifilm, Fumatech, and Suez were tested, and the results were compared. The unit was fed with synthetic hypersaline solution mimicking the concentration of natural bitterns (5 mol/L of NaCl) on one side, and with variable concentration of NaCl dilute solutions (0.01–0.1 mol/L) on the other. The influence of several op-erating parameters has also been assessed, including solutions flowrate and temperature. In-creasing feed solutions’ temperature and velocity has been found to lower the stack resistance, which enhances the output performance of the RED stack. The maximum obtained power density (corrected to account for the effect of electrodic compartments, which can be very relevant in five cell pairs laboratory stacks) reached around 10.5 W/m2cellpair, with FUJIFILM Type 10 membranes, temperature of 40 °C, and a fluid velocity of 3 cm s−1 (as empty channel, considering 270 m thickness). Notably, the present study results confirm the large potential for SGP generation from hypersaline brines, thus providing useful guidance for the harvesting of SGP in seawater saltworks all around the world.</p>
Mg(OH)2 Recovery from Real Bitterns: a Proof of Concept at Pilot Scale
<p>Water, energy, and minerals are fundamental pillars for the future of humankind. Sustainable and renewable productive processes and resources are the only possibility to face the continuously growing global population and high living standards requirements. The present work introduces a proof of concept for the pilot scale production of magnesium hydroxide, Mg(OH)<sub>2</sub>, from waste saltworks bitterns located in the district of Trapani, Italy. Mg(OH)<sub>2</sub> was produced by adopting a proprietary “Magnesium Crystals Granulometry Controlled Reactor”, Mg-CGCR. The influence of several parameters was investigated on Mg(OH)<sub>2</sub> suspensions and powders characteristics: (i) the bittern flow rate, (ii) alkaline sodium hydroxide, NaOH, concentrations solutions (adopted as the precipitant agent) and (iii) the final suspension pH value (stoichiometric or OH<sup>-</sup> excess amounts). A Mg<sup>2+</sup> recovery >99 % can be achieved thanks to the adoption of a product recycling strategy in the reactor. Furthermore, highly pure Mg(OH)<sub>2</sub> powders, addressed by cationic purity, were synthesized. Results demonstrate the possibility of producing highly pure Mg(OH)<sub>2</sub> products from waste-concentrated saline solutions, thus turning waste into valuable compounds.</p>
Characterization of Mg(OH)2 powders produced from real saltworks bitterns at a pilot scale
<p>The growing demand for a reliable supply of minerals has pushed the European Union toward seeking novel<br>mineral sources. In the present work, the recovery of magnesium, in the form of magnesium hydroxide, Mg<br>(OH)2, from saltworks bitterns was investigated at a pilot scale. The natural bittern collected from Margi saltworks<br>(Trapani, Italy) was treated with synthetic sodium hydroxide (NaOH) solutions. The influence of different<br>reactant concentrations, flow rates and pH environments, on Mg(OH)2 particle sizes, filtration characteristics,<br>Mg2+ extraction performance and the Mg(OH)2 solid purity was thoroughly assessed. The presence of additional<br>dissolved salts in NaOH solutions was also analyzed. The pH environment was found to be the most crucial<br>parameter. On the one hand, high pH values ensured high Mg2+ recovery and powder purities, i.e. > 98%, with<br>boron content complying with market requirements. On the other hand, filtration characteristics considerably<br>worsened due to the lyosorption phenomenon.</p>
Unlocking hidden mineral resources: Characterization and potential of bitterns as alternative sources of critical raw materials_dataset
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