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Keywords = copper basic salts

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18 pages, 6483 KiB  
Article
Surface Chemistry Aspects of Ion Exchange in Basic Copper Salts
by Sebastian Skupiński, Marta Kalbarczyk, Daniel Kamiński and Marek Kosmulski
Molecules 2025, 30(1), 21; https://doi.org/10.3390/molecules30010021 - 25 Dec 2024
Viewed by 289
Abstract
Brochantite was precipitated using stoichiometric amounts of CuSO4 and NaOH and characterized by scanning electron microscopy, specific surface area, thermogravimetric analysis, and zeta potential. Brochantite can be converted into paratacamite, basic copper bromide, and copper phthalate by shaking the powder with solutions [...] Read more.
Brochantite was precipitated using stoichiometric amounts of CuSO4 and NaOH and characterized by scanning electron microscopy, specific surface area, thermogravimetric analysis, and zeta potential. Brochantite can be converted into paratacamite, basic copper bromide, and copper phthalate by shaking the powder with solutions containing excess corresponding anions. By contrast, attempts to convert brochantite into basic iodide, acetate, nitrate, or rhodanide in a similar way failed, that is, the powder after shaking with solutions containing excess corresponding anions still showed the powder X-ray diffraction pattern of brochantite. Successful ion exchange resulted in a decrease in the specific surface area by a factor of 10, but the specific surface area was unchanged when attempts to exchange the anion failed. Interestingly enough, paratacamite can also be converted into brochantite by shaking with solution containing excess sulfate. Brochantite and paratacamite obtained by precipitation and the salts obtained by ion exchange showed a negative zeta potential at pH > 9. Full article
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Figure 1
<p>TGA curves of original brochantite (<b>A</b>) and paratacamite (<b>B</b>).</p>
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<p>SEM image of brochantite.</p>
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<p>SEM image of paratacamite.</p>
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<p>XRD pattern of brochantite. Line: experimental. Bars: from RRUFF repository.</p>
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<p>XRD pattern of paratacamite. Line: experimental. Bars: from RRUFF repository.</p>
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<p>Electrokinetic curves of the original brochantite.</p>
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<p>XRD patterns of B003, B005, B006 and B010. Lines: experimental. Bars: brochantite from RRUFF repository.</p>
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<p>XRD patterns of B001, B002, B007, and B008. Lines: experimental. Bars: brochantite from RRUFF repository.</p>
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<p>XRD patterns of B001, B008, and B012. Lines: experimental. Bars: atacamite (white) and paratacamite (black) from RRUFF repository.</p>
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<p>XRD patterns of B004, B014, and B015. Lines: experimental. Bars: brochantite from RRUFF repository.</p>
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<p>XRD patterns of B011, P017, and P018. Lines: experimental. Bars: brochantite (green) and paratacamite (black) from RRUFF repository.</p>
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<p>XRD patterns of P013 and P016. Lines: experimental. Bars: brochantite from RRUFF repository.</p>
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<p>Electrokinetic curves of B003, B005, B006, and B010.</p>
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<p>Electrokinetic curves of B001, B002, B007, B008, and B012.</p>
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<p>Electrokinetic curves of B004, B008, B014, and B015.</p>
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<p>Electrokinetic curves of B011, P017, and P018.</p>
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<p>Electrokinetic curves of P013 and P016.</p>
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17 pages, 2169 KiB  
Article
Study on Three-Stage Counter-Current Water Washing Desalination Characteristics and Mechanism of High Chlorine Waste Incineration Fly Ash
by Minjie Li, Jie Chen, Xiaoqing Lin, Tieying Mao, Zhongxu Zhu, Jiabao Lv, Congkai Fu, Siyu Chen, Angjian Wu, Xiaodong Li and Jianhua Yan
Processes 2022, 10(12), 2540; https://doi.org/10.3390/pr10122540 - 29 Nov 2022
Cited by 13 | Viewed by 2590
Abstract
The high chloride content of municipal solid waste incineration (MSWI) fly ash and hazardous waste incineration (HWI) fly ash has considerably affected their disposal. This study focused on investigating the three-stage counter-current (TSC) water-washing process to reduce the chlorine content efficiently under the [...] Read more.
The high chloride content of municipal solid waste incineration (MSWI) fly ash and hazardous waste incineration (HWI) fly ash has considerably affected their disposal. This study focused on investigating the three-stage counter-current (TSC) water-washing process to reduce the chlorine content efficiently under the premise of low water consumption. The liquid–solid ratio (LSR) and washing time were investigated, a chloride migration model was established, and the characteristics of the water-washing solution (WWS) and washed fly ash were investigated. The results showed that the dechlorination effect of TSC washing could reach more than 99% in a low liquid–solid ratio (LSR) of 2–4 kg/L. The most appropriate LSR and washing time were found to be around 3:1 L/kg and 15 min per stage, respectively. The concentration of Cl in WWS reached over 90 g/L, which is very high among industrial saline wastewater. Some heavy metals were also contained in the WWS, and lead was the main heavy metal, followed by zinc, copper, and arsenic. The concentration of WWS of different stages was calculated by a model, and the transfer characteristic of chloride was strongly related to the mass balance between the liquid contained in the solid–liquid separation residue (SR) and the separated liquid. After washing, due to the dissolution of soluble salt, the specific surface area of fly ash increased, and thus the absorption ability of the washed fly ash was greater than the raw one. This study provides a washing condition reference for highly chlorinated fly ash, the basic data of WWS, and the chloride migration model that is a preliminary calculation method to improve the water-washing process. Full article
(This article belongs to the Section Sustainable Processes)
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<p>XRD pattern of FA α.</p>
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<p>Circulating procedure and experimental procedure: (<b>a</b>) circulating procedure; (<b>b</b>) experimental procedure.</p>
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<p>Experimental devices.</p>
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<p>The concentration of Cl<sup>−</sup> of WWS obtained in different steps.</p>
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<p>The mass fraction of soluble chlorine in washed fly ash.</p>
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<p>The variation of the main components of simulated WWS.</p>
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<p>XRD diagram of precipitation.</p>
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21 pages, 3257 KiB  
Article
A Comprehensive Analysis of Selected Anionic Surfactants Behaviour in Aqueous Systems Containing Metal Ions and Inorganic Acid
by Anna Wołowicz, Katarzyna Staszak and Zbigniew Hubicki
Water 2022, 14(22), 3676; https://doi.org/10.3390/w14223676 - 14 Nov 2022
Cited by 5 | Viewed by 3846
Abstract
The influence of co-ions on the adsorption properties of two surfactants: ABS (dodecylbenzene sulfonic acid) and its sodium salt ABSNa50 in the aqueous systems, has been studied and discussed. On the basis of experimental measurements of equilibrium and dynamic surface tension, a series [...] Read more.
The influence of co-ions on the adsorption properties of two surfactants: ABS (dodecylbenzene sulfonic acid) and its sodium salt ABSNa50 in the aqueous systems, has been studied and discussed. On the basis of experimental measurements of equilibrium and dynamic surface tension, a series of parameters were determined, such as critical micelle concentration (CMC), adsorption parameters, diffusion coefficients, and the micellar dissociation constant. It was proved that values of CMC vary according the contents of accompanying metal ions (zinc(II), copper(II), cobalt(II), nickel(II)) and hydrochloric acid in the system under discussion. Moreover, it was found that as the concentration of surfactant in the system increases, the estimated values of the diffusion coefficients decrease. The obtained results indicate the need to analyse the basic surface properties of surfactants in case of their application in the systems containing additional substances. Full article
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<p>The adsorption isotherms for the ABS surfactant without (<bold>a</bold>) and with (<bold>b</bold>–<bold>f</bold>) heavy metals in water (<bold>a</bold>–<bold>e</bold>) and HCl (<bold>f</bold>) systems with constant concentration of heavy metal ions equal to 100 mg/L and effect of HCl concentration (<bold>g</bold>) as well as type of heavy metal ions (<bold>h</bold>) on <inline-formula><mml:math id="mm52"><mml:semantics><mml:mrow><mml:mi>CMC</mml:mi></mml:mrow></mml:semantics></mml:math></inline-formula> values.</p>
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<p>The adsorption isotherms for the ABS surfactant without (<bold>a</bold>) and with (<bold>b</bold>–<bold>f</bold>) heavy metals in water (<bold>a</bold>–<bold>e</bold>) and HCl (<bold>f</bold>) systems with constant concentration of heavy metal ions equal to 100 mg/L and effect of HCl concentration (<bold>g</bold>) as well as type of heavy metal ions (<bold>h</bold>) on <inline-formula><mml:math id="mm52"><mml:semantics><mml:mrow><mml:mi>CMC</mml:mi></mml:mrow></mml:semantics></mml:math></inline-formula> values.</p>
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<p>The <inline-formula><mml:math id="mm53"><mml:semantics><mml:mrow><mml:mi>CMC</mml:mi></mml:mrow></mml:semantics></mml:math></inline-formula> values comparison obtained for ABS (this paper) and ABSNa50 surfactants for systems without (<bold>a</bold>) and with (<bold>b</bold>–<bold>e</bold>) heavy metals such as Cu(II) (<bold>b</bold>), Co(II) (<bold>c</bold>), Ni(II) (<bold>d</bold>) and Zn(II) (<bold>e</bold>) [<xref ref-type="bibr" rid="B19-water-14-03676">19</xref>].</p>
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<p>ABS surfactant forms and mechanism of ABS adsorption in the aqueous solutions.</p>
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<p>2D Kernel density graph for (<bold>a</bold>) ABS and (<bold>b</bold>) ABSNa50 surfactants.</p>
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<p>Characterization of the parameters used for the ABS and ABSNa50 adsorption.</p>
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<p>Relations between the Γ<sup>∞</sup> versus concentration of surfactants: (<bold>a</bold>,<bold>d</bold>) ABSNa50 and (<bold>b</bold>,<bold>c</bold>) ABS in the presence of Cu(II) (<bold>a</bold>,<bold>b</bold>) and Zn(II) (<bold>c</bold>,<bold>d</bold>).</p>
Full article ">Figure 6 Cont.
<p>Relations between the Γ<sup>∞</sup> versus concentration of surfactants: (<bold>a</bold>,<bold>d</bold>) ABSNa50 and (<bold>b</bold>,<bold>c</bold>) ABS in the presence of Cu(II) (<bold>a</bold>,<bold>b</bold>) and Zn(II) (<bold>c</bold>,<bold>d</bold>).</p>
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<p>Plot of DST versus time for different anionic surfactant concentrations (water-ABS (<bold>a</bold>), water-ABSNa50 (<bold>b</bold>), 3 mol/L HCl-ABS (<bold>c</bold>), 3 mol/L HCl-ABSNa50 (<bold>d</bold>), 0.1 mol/L HCl-Co(II)-ABS (<bold>e</bold>), 0.1 mol/L HCl-Co(II)-ABSNa50 (<bold>f</bold>), 0.1 mol/L HCl-Cu(II)-ABSNa50 (<bold>g</bold>), 0.1 mol/L HCl-Ni(II)-ABSNa50 (<bold>h</bold>), 0.1 mol/L HCl-Zn(II)-ABSNa50 (<bold>i</bold>), 3 mol/L HCl-Zn(II)-ABSNa50 (<bold>j</bold>)) measured by the maximum bubble pressure methods—the selected examples (5 <inline-formula><mml:math id="mm54"><mml:semantics><mml:mrow><mml:mi>CMC</mml:mi></mml:mrow></mml:semantics></mml:math></inline-formula> ABS = 0.0063 mol/L, 5 <inline-formula><mml:math id="mm55"><mml:semantics><mml:mrow><mml:mi>CMC</mml:mi></mml:mrow></mml:semantics></mml:math></inline-formula> ABSNa50 = 0.0073 mol/L).</p>
Full article ">Figure 7 Cont.
<p>Plot of DST versus time for different anionic surfactant concentrations (water-ABS (<bold>a</bold>), water-ABSNa50 (<bold>b</bold>), 3 mol/L HCl-ABS (<bold>c</bold>), 3 mol/L HCl-ABSNa50 (<bold>d</bold>), 0.1 mol/L HCl-Co(II)-ABS (<bold>e</bold>), 0.1 mol/L HCl-Co(II)-ABSNa50 (<bold>f</bold>), 0.1 mol/L HCl-Cu(II)-ABSNa50 (<bold>g</bold>), 0.1 mol/L HCl-Ni(II)-ABSNa50 (<bold>h</bold>), 0.1 mol/L HCl-Zn(II)-ABSNa50 (<bold>i</bold>), 3 mol/L HCl-Zn(II)-ABSNa50 (<bold>j</bold>)) measured by the maximum bubble pressure methods—the selected examples (5 <inline-formula><mml:math id="mm54"><mml:semantics><mml:mrow><mml:mi>CMC</mml:mi></mml:mrow></mml:semantics></mml:math></inline-formula> ABS = 0.0063 mol/L, 5 <inline-formula><mml:math id="mm55"><mml:semantics><mml:mrow><mml:mi>CMC</mml:mi></mml:mrow></mml:semantics></mml:math></inline-formula> ABSNa50 = 0.0073 mol/L).</p>
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<p>Characterization of the parameters used for diffusion determination in the ABS and ABSNa50 adsorption [<xref ref-type="bibr" rid="B59-water-14-03676">59</xref>].</p>
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<p>Selected examples of approximation plots (short, long time) in the HCl–AS–M(II) systems where AS indicates ABS (<bold>a</bold>–<bold>d</bold>) and ABSNa50 (<bold>e</bold>,<bold>f</bold>) surfactants.</p>
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15 pages, 4603 KiB  
Article
Synthesis of Novel Aqua ƞ4-NNNO/Cu(II) Complexes as Rapid and Selective Oxidative Catalysts for O-Catechol: Fluorescence, Spectral, Chromotropism and Thermal Analyses
by Amjad M. Shraim, Kifah S. M. Salih, Ranim E. Al-Soufi, Soaad R. Al-Mhini, Mohammad I. Ahmad and Ismail Warad
Crystals 2021, 11(9), 1072; https://doi.org/10.3390/cryst11091072 - 4 Sep 2021
Cited by 7 | Viewed by 2764
Abstract
A new tetradentate Schiff base (SB), (E)-4-fluoro-2-(1-((2-(piperazin-1-yl)ethyl)imino)ethyl)phenol, was synthesized from condensation of 2-(1-piperazinyl)ethylamine and 5-fluoro-2-hydroxyacetophenone. This ligand was coordinated with three copper(II) salts (CuCl2, CuBr2 and Cu(NO3)2⸱3H2O) separately, giving rise to new neutral water-soluble [...] Read more.
A new tetradentate Schiff base (SB), (E)-4-fluoro-2-(1-((2-(piperazin-1-yl)ethyl)imino)ethyl)phenol, was synthesized from condensation of 2-(1-piperazinyl)ethylamine and 5-fluoro-2-hydroxyacetophenone. This ligand was coordinated with three copper(II) salts (CuCl2, CuBr2 and Cu(NO3)2⸱3H2O) separately, giving rise to new neutral water-soluble Cu(II)/ƞ4-NNNO complexes (13). The new materials were fully characterized by standard spectroscopic, elemental, thermal, electronic, absorption, and fluorescence analyses. The chromotropism investigation of the aqueous solutions of the complexes revealed notable outcomes. A turn off-on halochromism effect was observed, both in the acidic and basic mediums. The green-colored solution was changed to colorless (off) upon the addition of HCl, while the initial green color was reversibly restored (on) after the addition of NaOH. On the other hand, bathochromic solvatochromism shifts were noticed in various solvents. Interestingly, complex 2 displayed a remarkable blue fluorescence shift (Δλ = 90 nm) when compared to its SB ligand. The oxidation capability of the three complexes was successfully demonstrated for the conversion of o-catechol to o-benzoquinone in aqueous solutions and in the presence of H2O2, an environmentally friendly oxidant, under mild reaction conditions. Full article
(This article belongs to the Special Issue New Trends in Crystals at Saudi Arabia)
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<p><sup>1</sup>H- and <sup>13</sup>C-NMR of the SB-functionalized ligand in DMSO-<span class="html-italic">d</span><sub>6</sub>.</p>
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<p>FT-IR of 2-(1-piperazinyl)ethylamine (<b>a</b>), 5-fluoro-2-hydroxyacetophenone (<b>b</b>), ligand (<b>c</b>), complex <b>1</b> (<b>d</b>).</p>
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<p>SEM images for ligand (<b>a</b>) and complex <b>2</b> (<b>b</b>); EDX for ligand (<b>c</b>) and complex <b>2</b> (<b>d</b>).</p>
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<p>UV–Vis spectra of 2-(1-piperazinyl)ethylamine (<b>a</b>), 5-fluoro-2-hydroxyacetophenone (<b>b</b>), ligand (<b>c</b>), complex <b>1</b> (<b>d</b>), and complex <b>1</b> at a concentrated level (<b>e</b>).</p>
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<p>Emission spectra of 1 × 10<sup>−5</sup> M of ligand and complex <b>2</b> dissolved in DMSO at RT.</p>
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<p>Plot of absorbance of Cu(II)-L interaction at varying concentrations of Cu(II) (<b>a</b>); Job’s plot of Cu(II)-NNNO complex <b>1</b> at λ<sub>max</sub> = 620 nm (<b>b</b>).</p>
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<p>[H<sup>+</sup>]-dependent visible spectra of complex <b>1</b> in water at RT (<b>a</b>) and Abs. vs. [H<sup>+</sup>] relation at constant λ<sub>max</sub> = 625 nm (<b>b</b>).</p>
Full article ">Figure 8
<p>Solvatochromism of complex <b>2</b>: Abs. vs. λ<sub>max</sub> at LMCT (<b>a</b>) and at d-d (<b>b</b>), λ<sub>max</sub> vs. solvents DN/NA at LMCT (<b>c</b>) and at d-d (<b>d</b>).</p>
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<p>TGA (<b>a</b>) and DTG (<b>b</b>) of the tetradentate ligand and complex <b>2</b>.</p>
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<p>Electrolytic conductivity of complex <b>2</b>.</p>
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<p>(<b>a</b>) UV-Vis spectra of formation of 1,2-benzoquinone from o-catechol using complex <b>3</b> catalytic matrix, and (<b>b</b>) relation graph between absorbance at λ = 358 nm and time.</p>
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<p>Synthesis of SB-functionalized ligand and it complexes.</p>
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<p>Catalytic oxidation of o-catechol.</p>
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20 pages, 5318 KiB  
Review
Advances in Understanding of the Application of Unit Operations in Metallurgy of Rare Earth Elements
by Srecko Stopic and Bernd Friedrich
Metals 2021, 11(6), 978; https://doi.org/10.3390/met11060978 - 18 Jun 2021
Cited by 18 | Viewed by 6466
Abstract
Unit operations (UO) are mostly used in non-ferrous extractive metallurgy (NFEM) and usually separated into three categories: (1) hydrometallurgy (leaching under atmospheric and high pressure conditions, mixing of solution with gas and mechanical parts, neutralization of solution, precipitation and cementation of metals from [...] Read more.
Unit operations (UO) are mostly used in non-ferrous extractive metallurgy (NFEM) and usually separated into three categories: (1) hydrometallurgy (leaching under atmospheric and high pressure conditions, mixing of solution with gas and mechanical parts, neutralization of solution, precipitation and cementation of metals from solution aiming purification, and compound productions during crystallization), (2) pyrometallurgy (roasting, smelting, refining), and (3) electrometallurgy (aqueous electrolysis and molten salt electrolysis). The high demand for critical metals, such as rare earth elements (REE), indium, scandium, and gallium raises the need for an advance in understanding of the UO in NFEM. The aimed metal is first transferred from ores and concentrates to a solution using a selective dissolution (leaching or dry digestion) under an atmospheric pressure below 1 bar at 100 °C in an agitating glass reactor and under a high pressure (40–50 bar) at high temperatures (below 270 °C) in an autoclave and tubular reactor. The purification of the obtained solution was performed using neutralization agents such as sodium hydroxide and calcium carbonate or more selective precipitation agents such as sodium carbonate and oxalic acid. The separation of metals is possible using liquid (water solution)/liquid (organic phase) extraction (solvent extraction (SX) in mixer-settler) and solid-liquid filtration in chamber filter-press under pressure until 5 bar. Crystallization is the process by which a metallic compound is converted from a liquid into a crystalline state via a supersaturated solution. The final step is metal production using different methods (aqueous electrolysis for basic metals such as copper, zinc, silver, and molten salt electrolysis for REE and aluminum). Advanced processes, such as ultrasonic spray pyrolysis, microwave assisted leaching, and can be combined with reduction processes in order to produce metallic powders. Some preparation for the leaching process is performed via a roasting process in a rotary furnace, where the sulfidic ore was first oxidized in an oxidic form which is a suitable for the metal transfer to water solution. UO in extractive metallurgy of REE can be successfully used not only for the metal wining from primary materials, but also for its recovery from secondary materials. Full article
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<p>One combined hydrometallurgical and pyrometallurgical process for the production of rare earth elements.</p>
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<p>Signal flow in BP neural networks with four input neurons, nine hidden neurons, and one output neuron.</p>
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<p>Treatment of eudialyte concentrate using sulfuric acid.</p>
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<p>Treatment of eudialyte concentrate with hydrochloric acid at room temperature.</p>
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<p>(<b>a</b>) Acid digestion reactor and (<b>b</b>) system of two digestion reactor during operations (key elements: anchor stirrer, glass reactor (40 L), engine, an injected tube for a transport of suspension supported by a double membrane pump).</p>
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<p>(<b>a</b>) Two reactors for leaching (2 × 100 L), (<b>b</b>) System for leaching, neutralization, and filtration. Main components: neutralization unit (3 reactors × 10 L and 1 × 8.5 L), stirred collecting tank (250 L) and separation unit (chamber filter press).</p>
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<p>New developed dry digestion reactor (main components: reaction vessel, system with nozzles for injection of water and acid; cover; special mixing system, engine, discharging system, and electronics).</p>
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<p>Treatment of eudialyte concentrate by MEAB Chemie Technik GmbH and IME, RWTH Aachen.</p>
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<p>Treatment of bastnasite concentrate by MEAB Chemie Technik GmbH and IME, RWTH Aachen.</p>
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<p>Combined process for treatment of spent NdFeB-Magnets.</p>
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<p>Combined hydrometallurgical and pyrometallurgical method for production of yttrium oxide.</p>
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<p>A zero-waste valorization vision for bauxite residue through experimental results: (<b>a</b>) for cement industry (left), and (<b>b</b>) treatment of AMD solution and recovery of Fe, V, Ti, REE, and Sc (right).</p>
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11 pages, 2457 KiB  
Article
Synthesis of a New Polyanion Possessing Dense 1,2,3-Triazole Backbone
by Linlin Xu, Yuri Kamon and Akihito Hashidzume
Polymers 2021, 13(10), 1614; https://doi.org/10.3390/polym13101614 - 17 May 2021
Cited by 7 | Viewed by 2348
Abstract
Polyanions are an important class of water-soluble polymers because polyanions are utilized in a wide range of industrial fields. It is thus a great challenge to develop polyanions with novel structures to make their applications broader. In this study, a new polyanion with [...] Read more.
Polyanions are an important class of water-soluble polymers because polyanions are utilized in a wide range of industrial fields. It is thus a great challenge to develop polyanions with novel structures to make their applications broader. In this study, a new polyanion with a dense 1,2,3-triazole backbone, poly(4-azido-5-hexanoic acid) (poly(AH)), was synthesized by copper(I)-catalyzed azide–alkyne cycloaddition (CuAAC) polymerization of t-butyl 4-azido-5-hexanoate followed by hydrolysis of the t-butyl ester groups. Turbidimetric and potentiometric titration data indicated that poly(AH) was well soluble in water under basic conditions (pH < 7) and a weaker polyanion (apparent pKa = 5.4) than polyacrylic acid (apparent pKa = 4.5). Adsorption tests exhibited that sodium salt of poly(AH) (poly(AH)Na) adsorbed most preferably Fe3+ among the four metal ions examined, i.e., Cu2+, Pb2+, Li+, and Fe3+. 1H spin-lattice relaxation time measurements indicated that Fe3+ ions were adsorbed favorably onto the 1,2,3-triazole residues. Full article
(This article belongs to the Section Polymer Chemistry)
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Figure 1
<p><sup>1</sup>H NMR spectrum for poly(tBuAH) (CDCl<sub>3</sub>) (<b>a</b>) and poly(AH) (D<sub>2</sub>O) (<b>b</b>). Assignments are indicated as a, b, c, d, and e. Asterisks denote the signals due to the residual protons in solvents.</p>
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<p>FTIR spectrum for poly(tBuAH) (<b>a</b>) and poly(AH) (<b>b</b>).</p>
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<p>Turbidimetric and potentiometric titration data for an aqueous solution of poly(AH). The titration was performed by stepwise addition of 30 μL of 0.10 M HCl starting from pH 9.9.</p>
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<p>2D DOSY data for poly(AH)Na in D<sub>2</sub>O containing 5 mM NaCl at pH 9.0 (<b>a</b>) and 12.0 (<b>b</b>).</p>
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<p>Removal ratio of poly(AH)Na for Cu<sup>2+</sup>, Pb<sup>2+</sup>, Li<sup>+</sup>, and Fe<sup>3+</sup>.</p>
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<p><sup>1</sup>H NMR spectrum for poly(AH)Na in the absence (<b>a</b>) and presence of 0.1 (<b>b</b>), 3.1 (<b>c</b>), and 9.1 mM of Fe(NO<sub>3</sub>)<sub>3</sub> (D<sub>2</sub>O) (<b>d</b>). Assignments are indicated as a, b, c, and d. Asterisks denote the signals due to the residual protons in solvents.</p>
Full article ">Figure 7
<p><span class="html-italic">T</span><sub>1,pAHFe</sub>/<span class="html-italic">T</span><sub>1,pAH</sub> for <sup>1</sup>H NMR signals.</p>
Full article ">Scheme 1
<p>Synthesis of poly(AH) by CuAAC polymerization of tBuAH followed by hydrolysis of the <span class="html-italic">t</span>-Bu ester.</p>
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13 pages, 3182 KiB  
Communication
Easy, Quick, and Reproducible Sonochemical Synthesis of CuO Nanoparticles
by Nataly Silva, Sara Ramírez, Isaac Díaz, Andreina Garcia and Natalia Hassan
Materials 2019, 12(5), 804; https://doi.org/10.3390/ma12050804 - 8 Mar 2019
Cited by 74 | Viewed by 6692
Abstract
Copper oxide nanoparticles (CuO NPs) were synthesized in air by reducing copper (II) sulfate pentahydrate salt (CuSO4·5H2O) in the presence of sodium borohydride. The reaction was stabilized with Hexadecyltrimethylammonium bromide (CTAB) in a basic medium and using ultrasound waves. [...] Read more.
Copper oxide nanoparticles (CuO NPs) were synthesized in air by reducing copper (II) sulfate pentahydrate salt (CuSO4·5H2O) in the presence of sodium borohydride. The reaction was stabilized with Hexadecyltrimethylammonium bromide (CTAB) in a basic medium and using ultrasound waves. Different molar ratios of CTAB:Cu2+ and NaBH4:Cu2+ were explored, to optimize the synthesis conditions, and to study the stability, size, and Zeta potential of the colloidal suspension. Optimum conditions to generate spherical, stable, and monodispersed nanoparticles with hydrodynamic diameters of 36 ± 1.3 nm were obtained, using 16 mM CTAB and 2 M NaBH4 (molar ratios Cu2+:CTAB:NaBH4 of 1:6:10). X-ray diffraction (XRD) was implemented, and a monoclinic CuO crystal system was formed. This demonstrated a monoclinic crystal system corresponding to CuO. The diffraction peaks were identified and confirmed according to their selected area electron diffraction (SAED) patterns. Full article
(This article belongs to the Special Issue Fabrication of 1D and 2D Nanomaterials)
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Figure 1

Figure 1
<p>Evolution UV-Vis spectra of the colloidal suspensions recorded over 20 hr. Spectra were recorded at 20 °C between 300 and 850 nm, measured every 15 min. The insert shows a photograph of a glass vial that is similar to the colored colloidal suspension.</p>
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<p>Transmission Electron Microscopy (TEM) micrographs of (<b>a</b>) copper nanoparticle (Cu NPs) and (<b>b</b>) copper oxide nanoparticle (CuO NPs) with their respective particle size distribution histograms.</p>
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<p>(<b>a</b>) X-ray powder diffraction patterns of CuO NPs and CTAB. (<b>b</b>) Selected areas of electron diffraction of CuO NPs. (<b>c</b>) HR-TEM and (<b>d</b>) Fast Fourier Transform (FFT) of CuO NPs.</p>
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<p>Schematic representation of the synthesis mechanism of CuO NPs obtained by the sonochemical method. Step I: CTAB micelle in basic solution (uncolored). Step II: Suspension of copper hydroxide (light -blue coloration). Step III: Reduction of Cu(OH)<sub>2</sub> and Cu<sup>2+</sup> by the synergic effects of NaBH<sub>4</sub> and H<sub>2,</sub> generating nuclei that contain small Cu NPs formed in the periphery of the micelle (dark brown suspension). Step IV: Nucleation by the oxidation of Cu NPs, and structural micellar rearrangement. The CTAB micelles cap the CuO NPs after they are formed (yellow colloidal suspension).</p>
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