Search Results (115)

Rare earth metals (REMs) are vital for high-tech industries, but their extraction from secondary sources is challenging due to environmental and technical constraints. This study investigates the ion-exchange extraction of light REMs (neodymium, praseodymium, and samarium) from sulfuric and phosphoric acid solutions, modeling industrial leachates from apatite concentrates and phosphogypsum. The study considers the use of anion- and cation-exchange resins with different functional groups for efficient and environmentally safe REM separation. Experimental sorption isotherms were obtained under static conditions at 298 K and analyzed using a thermodynamic model based on the linearization of the mass action equation. Equilibrium constants and Gibbs energy were calculated, which reveals the spontaneity of the processes. Cation-exchange resins demonstrated high selectivity towards individual REMs, while anion-exchange resins were suitable for group extraction. Infrared spectral analysis confirmed the presence of sulfate and phosphate complexes in the resin matrix, clarifying the ion-exchange mechanisms. Thermal effect measurements indicated exothermic sorption on anion-exchange resins with negative entropy and endothermic sorption on cation-exchange resins with positive entropy. The findings highlight the potential of ion-exchange resins for selective and sustainable REM recovery, offering a safer alternative to liquid extraction and enabling the valorization of industrial wastes like phosphogypsum for resource recovery. Full article

Industrial technologies for processing tungsten concentrates using soda roasting or autoclave leaching are based on the production of alkaline sodium tungstate solutions that contain impurities such as silicon, phosphorus, arsenic, and others. The purification of these solutions from impurities requires the neutralization of excess soda or alkali with inorganic acids, which leads to the formation of chloride and sulfate effluents that are subsequently discharged into waste repositories. An analysis was carried out on existing methods for the production and processing of sodium tungstate solutions using HNO₃ and NH₃, as well as extraction and sorption techniques involving anion exchange resins. Currently, processes such as nanofiltration, reverse osmosis, and electrodialysis are being applied for water purification and the treatment of sulfate and chloride effluents. These processes employ various types of industrially manufactured membranes. For the purpose of electrodialysis, a two-compartment electrodialyzer setup was employed using cation-exchange membranes of the MK-40 (Russia) and EDC1R (China) types. The composition and structure of sodium tungstate, used as the starting reagents, were analyzed. Based on experiments conducted on a laboratory-scale unit with continuous circulation of the catholyte and anolyte, dependencies of various parameters on current density and process duration were established. Stepwise changes in the anolyte pH were recorded, indirectly confirming changes in the composition of the Na₂WO₄ solution, including the formation of polytungstates of variable composition and the production of H₂WO₄ via electrodialysis at pH < 2. The resulting tungstic acid solutions were also analyzed. The conducted studies on the processing of sodium tungstate solutions using electrodialysis made it possible to obtain alkaline solutions and tungstic acid at a current density of 500–1500 A/m², without the use of acid for neutralization. Yellow tungstic acid was obtained from the tungstic acid solution by evaporation. Full article

Fructooligosaccharides (FOSs) are carbohydrates of high nutritional value with various prebiotic properties. Optimizing their production process is of significant interest for expanding commercial-scale production. This review discusses the properties and potential applications of FOSs, addressing production challenges and providing an economic market analysis. Bibliometric analysis of data concerning the functional properties, production, purification, and applications of FOSs revealed an over 87% increase in the number of worldwide publications from 2012 to 2022, rising from 88 to 165. Furthermore, contributions from ninety-three countries were identified up to 2024, with Brazil ranking first, with 326 publications. Furthermore, Aureobasidium sp. and Aspergillus sp. have shown the best results for FOS production, with reported conversion in the order of 0.66 g FOS/g sucrose. Nevertheless, the formation of by-products or co-products requiring separation from the medium remains a challenge. Activated carbon, cation exchange resins, and zeolites are highlighted as key adsorbents, with the adsorption process achieving FOS purity exceeding 90%. Furthermore, membrane technology is identified as a more efficient and promising separation method. Addressing these limitations will facilitate the further expansion of the growing global FOS market, promoting a sustainable approach and their integration with biorefineries, which can enable the development of a wider range of value-added products. Full article

A membrane system was applied for ultrapure water production from the treatment of saline effluent from the canned food industry. The industrial effluent presented a high saline concentration, including sodium chloride, calcium carbonate, calcium sulfates, and magnesium. The effluent was treated using a system of reverse osmosis (RO) and a post-treatment process consisting of ion exchange resins (IEXRs). The RO was accompanied by the addition of a hexametaphosphate dose (2, 6, and 10 mg/L) as an antiscalant to avoid the RO membrane scaling by minerals. In turn, IEXRs were used for water deionization to produce ultrapure water with a reduced concentration of monovalent ions. The antiscalant dose was 6 mg/L, producing clean water from RO permeates with an efficiency of 65–70%. The brine from RO was projected for its reuse in food industry processes. The clean water quality from RO showed 20% total dissolved solids (TDS) removal (equivalent to salts). The antiscalant inhibited the formation of calcium salt incrustation > 200 mg/L, showing low fouling. In turn, anionic resins removed 99.8% of chloride ions, whereas the monovalent salts were removed by a mix of cationic–anionic resin, producing ultrapure water with electrical conductivity < 3.3 µS/cm. The cost of ultrapure water production was 2.62 USD/m³. Full article

Reverse osmosis concentrate (ROC) treatment is critical for enhancing water recovery and minimizing concentrate volume for disposal, especially in regions facing water scarcity. This study investigates the application of ion exchange (IX) resins and activated alumina (AA) as pretreatment strategies to mitigate scaling in ROC due to high concentrations of total dissolved solids, hardness (Ca²⁺ and Mg²⁺), and silica. Through a series of Langmuir isotherms, continuous column experiments, and model simulation, two types of strong acid cation IX resins and three types of strong base anion IX resins alongside three types of AA were evaluated. Results indicate that AA exhibits superior performance in silica removal, achieving up to a 65% reduction and maintaining performance for up to 800 bed volume without reaching saturation. Model simulation of a secondary reverse osmosis treating ROC after the IX and AA pretreatment indicated an additional water recovery of ~70% using antiscalants. This study demonstrates the potential for achieving higher water recovery while also identifying opportunities for pretreatment improvement. Challenges such as the limited IX capacity treating ROC, which requires frequent regeneration and increases operational costs, along with the restricted regeneration capacity of AA, underscore the importance of innovation. These findings emphasize the critical need for developing advanced materials and optimized strategies to further enhance the efficiency of ROC treatment processes. Full article

The efficiency of integrated treatment systems for wastewater generated during the washing of disinfectant production lines was investigated. The high organic load (COD 2000 mg/L, TOC 850 mg/L) and 300 mg/L of toxic benzalkonium chloride (BAC) make wastewater an environmental hazard that requires advanced treatment. Initial tests on model BAC solutions (in concentrations corresponding to those found in wastewater), using nanofiltration and ultrafiltration membranes, resulted in up to 70% retention of BAC. To enhance purification, ion exchange and adsorption were introduced as post-membrane treatment steps. In the second part of the investigation, membrane modules characterized by the best separation properties were integrated together with macroporous cation-exchange resin and activated carbon into the purification system to treat wastewater. The research carried out showed that the purification of multicomponent wastewater is a complex task. Significantly lower BAC removal (30%) was achieved in membrane processes compared to the model solutions treatment. In integrated systems, the BAC concentration was reduced to 100 mg/L, TOC to 200 mg/L, and COD to 120 mg/L. Full article

The gradual increase in water scarcity due to depletion and/or inadequate use of water resources has affected the automotive sector. In this context, possibilities for water reuse in the pre-treatment tunnel in an automotive painting process were studied and compared with the primary goal of finding the most appropriate and economically viable water recovery solutions, considering a circular economy metric approach. To this end, an experimental campaign of aqueous effluent characterization, with determinations of most relevant chemical and physical parameters, was conducted in a company in the automotive industry sector. To reduce alkalinity and remove surfactants from the effluent of the washing phase, a cation exchange on a weak-acid-based resin was proposed along with a microfiltration membrane system with a recovery efficiency of 88%. The inclusion of subsequent ultrafiltration and reverse osmosis steps proved to be the most suitable for removing salts and biocides from the water of the cooling towers, treating approximately 68% of the water. The techno-economic feasibility was comprehensively evaluated according to the type of treatment used. A cost of EUR 245 thousand was estimated for the treatment of water from the degreasing washing phase (EUR 1.06 per manufactured car), and a cost of EUR 582 thousand was estimated for the treatment of the cooling towers’ water (EUR 2.52 per car). The estimated water income after the treatment systems’ implementation was estimated to be equal to EUR 0.07 per car for the washing stage and EUR 0.13 per car for the cooling towers. Ultimately, this study clearly demonstrated the beneficial contribution of using membrane treatment in the automotive sector’s environmental policy, leading to water reuse and much lower effluent discharge according to the principles of the circular economy. Full article

Sinapine adsorption was studied on four weak cation exchanges at pHs ranging from 2 to 8. The best adsorption rate was observed with C106 resin at pH 4 (95.25%). The adsorption kinetics followed a pseudo-second-order model while the isotherm data better fitted the Langmuir model. The ΔG°, ΔH°, and ΔS° values (−25.834 kJ·mol⁻¹, −24.428 kJ·mol⁻¹, and 0.004 kJ·mol⁻¹·K⁻¹) revealed that the adsorption process was spontaneous and exothermic. Acidified ethanol showed a better desorption rate (75.41%), while virtually no (3.32%) or low (31.14%) sinapine desorption was observed with 50% ethanol and 0.1 M HCl solution, respectively. This indicated that sinapine adsorption took place throughout both ionic and hydrophobic interactions. Very close sinapine adsorption performances were observed with an effluent of the patented rapeseed protein isolate process. Two-step desorption using 50% ethanol, then acidified ethanol, yielded a highly purified neutral sinapine-derivative phenol fraction (75.23%) in the first elution fraction and sinapine (98.85%) in the second one. Full article

The contamination of water by heavy metals poses an escalating risk to human health and the environment, underscoring the critical need for efficient removal methods to secure safe water resources. This study evaluated the performance of four cationic exchange materials (labeled “PS—DVB”, “PA—DVB”, “TFSA”, and “OGL”) in removing or harvesting metals such as copper, silver, lead, cobalt, and nickel from aqueous solutions, several of which are precious and/or classified as Critical Raw Materials (CRMs) due to their economic importance and supply risk. The objective was to screen and benchmark the four ion exchange materials for water treatment applications by investigating their metal sequestration capacities. Experiments were conducted using synthetic solutions with controlled metal concentrations, analyzed through ICP-OES, and supported by kinetic modeling. The adsorption capacities (qe) obtained experimentally were compared with those predicted by pseudo-first-order and pseudo-second-order models. This methodology enables high precision and reproducibility, validating its applicability for assessing ion exchange performance. The results indicated that PS—DVB and PA—DVB resins proved to be of “wide range”, exhibiting high efficacy for most of the metals tested, including CRM-designated ones, and suggesting their suitability for water purification. Additionally, the second-life Nafion-based “TFSA” material demonstrated commendable performance, highlighting its potential as a viable and technologically advanced alternative in water treatment. Lastly, the lignin-based material, “OGL”, representing the most innovative and sustainability apt option, offered relevant performance only in selected cases. The significant differences in performance among the resins underscore the impact of structural and compositional factors on adsorption efficiency. This study offers valuable insights for investigating and selecting new sustainable materials for treating contaminated water, opening new pathways for targeted and optimized solutions in environmental remediation. Full article

Background: N-succinimidyl-[¹⁸F]fluorobenzoate ([¹⁸F]SFB) is commonly prepared through a three-step procedure starting from [¹⁸F]fluoride ion. A number of methods for the single-step radiosynthesis of [¹⁸F]SFB have been introduced recently, including the radiofluorination of diaryliodonium salts and the Cu-mediated ¹⁸F-fluorination of pinacol aryl boronates and aryl tributyl stannanes, but they still have the drawbacks of lengthy product purification procedures. In the present work, two approaches for the direct labeling of [¹⁸F]SFB from diaryliodonium (DAI) salt (4) and pinacol aryl boronate (6) are evaluated, with a major focus on developing a fast and simple SPE-based purification procedure. Methods: DAI salt precursor 6 was labeled employing the common “minimalist” approach with a two-step reaction heating sequence. The Cu-mediated radiofluorination of 4 was accomplished using Bu₄NOTf as a phase transfer catalyst for the elution of [¹⁸F]fluoride, followed by radiofluorination in the same solvent. Several types of SPE cartridges were tested in the elution and SPE procedures. Results: The Cu-mediated ¹⁸F-fluorination of the pinacol aryl boronate precursor afforded a higher RCC of 56 ± 3% (n = 7), making it better suited for the one-pot synthesis of [¹⁸F]SFB. SPE-based purification was achieved using cation exchange and reverse-phase polymer resin cartridges, connected in series. In a full-batch test, [¹⁸F]SFB was obtained with an RCY of 30% (n. d. c.), RCP > 99%, A_m 96–155 GBq/µmol, and a synthesis time of ≤35 min. Conclusions: Compared to other published methods, [¹⁸F]SFB production via the Cu-mediated radiofluorination of pinacol aryl boronate precursor provides significant time and cost savings, coupled with an ease of implementation. Full article

Host cell proteins (HCPs) are one of the process-related impurities that need to be well characterized and controlled throughout biomanufacturing processes to assure the quality, safety, and efficacy of monoclonal antibodies (mAbs) and other protein-based biopharmaceuticals. Although ELISA remains the gold standard method for quantification of total HCPs, it lacks the specificity and coverage to identify and quantify individual HCPs. As a complementary method to ELISA, the LC-MS/MS method has emerged as a powerful tool to identify and profile individual HCPs during the downstream purification process. In this study, we developed a sensitive, robust, and reproducible analytical flow ultra-high-pressure LC (UHPLC)-high-resolution accurate mass (HRAM) data-dependent MS/MS method for HCP identification and monitoring using an Orbitrap Ascend BioPharma Tribrid mass spectrometer. As a case study, the developed method was applied to an in-house trastuzumab product to assess HCP clearance efficiency of the newly introduced POROS™ Caprylate Mixed-Mode Cation Exchange Chromatography resin (POROS Caprylate mixed-mode resin) by monitoring individual HCP changes between the trastuzumab sample collected from the Protein A pool (purified by Protein A chromatography) and polish pool (purified by Protein A first and then further purified by POROS Caprylate mixed-mode resin). The new method successfully identified the total number of individual HCPs in both samples and quantified the abundance changes in the remaining HCPs in the polish purification sample. Full article

The effective recovery of gallium from wastewater discharge in the Bayer process is promising for the long-term development of gallium resources. The adsorption and desorption behavior of gallium (Ga), vanadium (V), and aluminum (Al) ions on a strong acidic styrene cation exchange resin (JK resin) from a simulated Bayer solution was systematically investigated by static experiments. The results showed that the optimum conditions for separating Ga from V and Al were at low temperatures and short contact times, with 78.30%, 15.16%, and 6.63% of the adsorption efficiency at 25 °C and 60 min, respectively, for Ga, V, and Al. The adsorption kinetics of Ga³⁺ conformed to the pseudo-second order model, and the static saturation adsorption capacity was 18.25 mg/g. The Langmuir model fitted the adsorption isotherm of gallium well, and the maximum adsorption capacity was 1.11 mg/g at 25 °C. FT-IR spectroscopy and XPS showed that the mechanism of the Ga³⁺ adsorption was only related to the interaction of the oxygen atoms of the amide oxime group (C=NOH). The separation of Ga, V, and Al can be achieved by desorbing 98% of Al with low concentrations of ammonia and 90% of Ga with low concentrations of hydrochloric acid. The results indicate that JK resin is an efficient adsorbent for separating gallium and vanadium in alkaline solutions. Full article

As the most abundant bioenergy raw material in nature, cellulose can be converted into sugar by hydrolysis, which can be further degraded to produce downstream chemicals, such as polyols. Hydrolysis technology is one of the key steps in the development and utilization of cellulosic biomass resources. In this study, the ionic liquid (IL)-catalyzed hydrolysis of sugarcane cellulose into reducing sugar was studied. Firstly, the hydrolysis of sugarcane cellulose in different ionic liquids (including benzothiazolomethane sulfonate, [HBth][CH₃SO₃] and 1-methyl-3-(3-sulfopropyl)-imidazolium hydrogen sulfate, [C₃SO₃Hmim]HSO₄) in heterogeneous and homogeneous systems to produce reducing sugar was studied. In a homogeneous system, the catalytic effect of an ionic liquid on sugarcane cellulose was explored. The pretreatment, IL dosage (0.1~1.0 g), reaction temperature (100~180 °C), addition of water (0~500 μL), and time (1~6 h) were all discovered as key conditions for hydrolysis. The acidity of an acidic ionic liquid is a key factor affecting the hydrolysis of sugarcane cellulose; meanwhile, effective pretreatment and water are also important. As a comparison, the catalytic effect of [C₃SO₃Hmim]HSO₄ in heterogeneous systems (the maximum yield of 5.98% for total reducing sugars, TRS) was not as good as that of [HBth][CH₃SO₃] in homogeneous systems (33.97%). A higher temperature does not necessarily lead to an increased TRS yield, but it will make the maximum TRS appear earlier. At last, 732 cationic ion exchange resin was used to investigate the separation of reducing sugar and ionic liquid, and the recovery of ionic liquid was investigated by an adsorption–desorption experiment. The ionic liquid can be well separated from TRS in the [HBth][CH₃SO₃] and reused at least five times. Full article

In order to systematize and expand knowledge about copper-containing composite materials as hybrid ion exchangers, in this study, fine metallic copper particles were dispersed within the matrix of a carboxyl cation exchanger (CCE) with a macroporous and gel-type structure thanks to the reduction of Cu₂O particles precipitated within the matrix earlier. It was possible to introduce as much as 22.0 wt% Cu⁰ into a gel-type polymeric carrier (G/H#Cu) when an ascorbic acid solution was used to act as a reducer of Cu₂O and a reagent transforming the functional groups from Na⁺ into the H⁺ form. The extremely high shrinkage of the porous skeleton containing –COOH groups (in a wet and also dry state) and its limited affinity for water protected the copper from oxidation without the use of special conditions. When macroporous CCE was used as a host material, the composite material (M/H#Cu) contained 18.5 wt% Cu, and copper particles were identified inside the resin beads, but not on their surface where Cu²⁺ ions appeared during drying. Thermal analysis in an air atmosphere and under N₂ showed that dispersing metallic copper within the resin matrix accelerated its decomposition in both media, whereby M/H#Cu decomposed faster than G/H#Cu. It was found that G/H#Cu contained 6.0% bounded water, less than M/H#Cu (7.5%), and that the solid residue after combustion of G/H#Cu and M/H#Cu was CuO (26.28% and 22.80%), while after pyrolysis the solid residue (39.35% and 26.23%) was a mixture of carbon (50%) and metallic copper (50%). The presented composite materials thanks to the antimicrobial, catalytic, reducing, deoxygenating and hydrophobic properties of metallic copper can be used for point-of-use and column water/wastewater treatment systems. Full article

Cation exchange resin (CER) has been reported to promote sludge fermentation. However, previous studies have typically focused on the effects of CER on sludge properties to enhance fermentation, and the role of CER as a biocarrier for anaerobic consortia during fermentation has been overlooked. Thus, in this study, the potential of gel-type and macro-reticular type CERs to serve as biocarriers in fermentation was investigated. A significant number of anaerobes appeared to be attached to the surfaces of CER during 2-day fermentation. However, an extended fermentation time negatively affected the attachment of anaerobic consortia, suggesting that CER may be a suitable carrier for short-term fermentation processes, such as biohydrogen fermentation. Electrochemical analyses revealed that the electron transfer capacities of CER with attached anaerobes were enhanced after both 2-day and 28-day fermentation periods, with the macro-reticular type CER exhibiting higher electron transfer capacity than the gel-type CER. Fermentation experiments using mixing model substrates with macro-reticular and gel-type CERs with attached anaerobes showed that the macro-reticular type CER was more beneficial for biohydrogen fermentation than the gel-type CER. Further analyses of microbial communities revealed that hydrogen-producing bacteria (i.e., Caloramator, unclassified_f_Caloramatoraceace, and Sporanaerobacter) were more likely to adhere to the macro-reticular type CERs. This outcome confirmed that macro-reticular type CERs have significant potential as a carrier for anaerobic consortia to promote the generation of hydrogen and volatile fatty acids. These findings are expected to provide a reference for using materials as biocarriers to enhance the biohydrogen fermentation of sludge. Full article