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Keywords = acid washing and calcining

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23 pages, 3249 KiB  
Article
Process Optimization and Performance Characterization of Preparing 4A Molecular Sieves from Coal Gangue
by Dongpeng Zhang, Laiyang Zhu, Tiantian Ma, Xiwen Liang, Nie Sun and Fei Liu
Symmetry 2025, 17(4), 603; https://doi.org/10.3390/sym17040603 - 16 Apr 2025
Cited by 1 | Viewed by 505
Abstract
Coal mining and washing processes generate substantial amounts of coal gangue, posing significant environmental challenges. Coal gangue as a solid waste is rich in SiO2 and Al2O3, with the SiO2/Al2O3 molar ratio closely [...] Read more.
Coal mining and washing processes generate substantial amounts of coal gangue, posing significant environmental challenges. Coal gangue as a solid waste is rich in SiO2 and Al2O3, with the SiO2/Al2O3 molar ratio closely aligned with the ideal composition of 4A molecular sieves. In this study, through a synergistic pretreatment process involving low-temperature oxidation and hydrochloric acid leaching, the Fe2O3 content in coal gangue was reduced from 7.8 wt% to 1.1 wt%, markedly enhancing raw material purity. The alkali fusion–hydrothermal synthesis parameters were optimized via orthogonal experiments—calcination (750 °C, 2 h), aging (60 °C, 2 h), and crystallization (95 °C, 6 h) to maintain cubic symmetry, yielding highly crystalline 4A zeolite. Characterization via XRD, calcium ion adsorption capacity, SEM, and FTIR elucidated the regulatory mechanism of calcination on kaolinite phase transformation and the critical role of alkali fusion in activating silicon–aluminum component release. The as-synthesized zeolite exhibited a cubic morphology, high crystallinity, and sharp diffraction peaks consistent with the 4A zeolite phase. The pH of the zero point charge (pHZPC) of the 4A molecular sieve is 6.13. The 4A molecular sieve has symmetry-driven adsorption sites, and the adsorption of Cu2+ follows a monolayer adsorption mechanism (Langmuir model, R2 = 0.997) with an average standard enthalpy change of 38.96 ± 4.47 kJ/mol and entropy change of 0.1277 ± 0.0148 kJ/mol, adhering to pseudo-second-order kinetics (R2 = 0.999). The adsorption process can be divided into two stages. This study provides theoretical and technical insights into the high-value utilization of coal gangue. Full article
(This article belongs to the Section Chemistry: Symmetry/Asymmetry)
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21 pages, 5085 KiB  
Article
Towards Achieving Circular Economy in the Production of Silica from Rice Husk as a Sustainable Adsorbent
by Alba Rodriguez-Otero, Anne Galarneau, Méghane Drané, Vicmary Vargas, Victor Sebastian, Andrew Wilson, David Grégoire, Sadia Radji, Frederic Marias, Jan H. Christensen and Brice Bouyssiere
Processes 2024, 12(11), 2420; https://doi.org/10.3390/pr12112420 - 2 Nov 2024
Cited by 3 | Viewed by 2750
Abstract
The growing concern over water pollution and waste management requires innovative solutions that promote resource efficiency within a circular economy. This study aims to utilize rice husk (RH) as a sustainable feedstock to develop highly porous silica particles and generate valuable by-products, addressing [...] Read more.
The growing concern over water pollution and waste management requires innovative solutions that promote resource efficiency within a circular economy. This study aims to utilize rice husk (RH) as a sustainable feedstock to develop highly porous silica particles and generate valuable by-products, addressing the dual challenges of waste reduction and water contamination. We hypothesize that optimizing the production of amorphous silica from acid-washed RH will enhance its adsorptive properties and facilitate the concurrent generation of bio-oil and syngas. Amorphous silica particles were extracted from acid-washed RH with a yield of 15 wt% using a combination of acid washing at 100 °C, pyrolysis at 500 °C, and calcination at 700 °C with controlled heating at 2 °C/min. The optimized material (RH2-SiO2), composed of small (60–200 nm) and large (50–200 µm) particles, had a specific surface area of 320 m2/g, with funnel-shaped pores with diameters from 17 nm to 4 nm and showed a maximum cadmium adsorption capacity of 407 mg Cd/g SiO2. Additionally, the pyrolysis process yielded CO-rich syngas and bio-oil with an elevated phenolic content, demonstrating a higher bio-oil yield and reduced gas production compared to untreated RH. Some limitations were identified, including the need for bio-oil upgrading, further research into the application of RH2-SiO2 for wastewater treatment, and the scaling-up of adsorbent production. Despite the challenges, these results contribute to the development of a promising adsorbent for water pollution control while enhancing the value of agricultural waste and moving closer to a circular economy model. Full article
(This article belongs to the Section Sustainable Processes)
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18 pages, 5507 KiB  
Article
Removal of Cd2+ and Pb2+ from an Aqueous Solution Using Modified Coal Gangue: Characterization, Performance, and Mechanisms
by Zhibing Chang, Chunwei Lu, Lu Bai, Nan Guo, Zhenguo Xing and Yinuo Yan
Processes 2024, 12(10), 2095; https://doi.org/10.3390/pr12102095 - 26 Sep 2024
Viewed by 1050
Abstract
The impact of various modification methods on enhancing the adsorption performance of coal gangue (CG) for hazardous heavy metals has not been thoroughly investigated. In this study, three CG samples were first modified by calcination, followed by acid washing, alkali washing, and hydrothermal [...] Read more.
The impact of various modification methods on enhancing the adsorption performance of coal gangue (CG) for hazardous heavy metals has not been thoroughly investigated. In this study, three CG samples were first modified by calcination, followed by acid washing, alkali washing, and hydrothermal treatment, to obtain modified CG samples. The adsorption performance was assessed based on the adsorption capacities for Cd2⁺ and Pb2⁺ (i.e., qe,Cd and qe,Pb), and the kinetics of the adsorption processes were analyzed using kinetic equations. XRD, SEM-EDX, FTIR, and N2 adsorption–desorption isotherms were used to elucidate the adsorption mechanisms. Results indicated that qe,Cd and qe,Pb of raw CG samples were approximately 10 and 25 mg/g, respectively, with only slight changes observed after calcination, acid washing, and alkali washing. In contrast, hydrothermal treatment yielded NaP and NaA zeolites, which significantly enhanced qe,Cd and qe,Pb to values of 48.5–72.7 and 214.9–247.5 mg/g, respectively. The hydrothermally treated CG samples primarily adsorbed Cd2⁺ and Pb2⁺ through ion exchange with Na⁺ within the zeolite structure, facilitating the entry of these ions into the zeolite’s pore channels. The adsorption processes were effectively described by the pseudo-second-order kinetic model. By optimizing the conditions of hydrothermal modification, the adsorption performance of CG samples is anticipated to further improve due to the creation of additional adsorption sites. Full article
(This article belongs to the Section Separation Processes)
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14 pages, 2117 KiB  
Article
Utilizing Nano-Adsorbents and Electrostatic Field Treatment for Sustainable Refinement of Crude Canola Oil
by Li Zhou, Timothy J. Tse, Farley Chicilo, Jianheng Shen, Venkatesh Meda and Martin J. T. Reaney
Foods 2024, 13(17), 2707; https://doi.org/10.3390/foods13172707 - 27 Aug 2024
Cited by 1 | Viewed by 1848
Abstract
Removal of polar impurities, such as phospholipids, free fatty acids (FFA), and peroxides, can be challenging during the refining of crude canola oil. Current conventional refining methods are energy-intensive (e.g., hot water washes) and can generate significant waste (e.g., wastewater effluent) and neutral [...] Read more.
Removal of polar impurities, such as phospholipids, free fatty acids (FFA), and peroxides, can be challenging during the refining of crude canola oil. Current conventional refining methods are energy-intensive (e.g., hot water washes) and can generate significant waste (e.g., wastewater effluent) and neutral oil loss. This study investigated the joint use of nano-adsorbents and electrostatic field (E-field) treatment as a potential and sustainable alternative in removing these impurities during the oil refining process. Specifically, aluminum oxide (Al2O3) nanoparticles were employed to neutralize FFAs, achieving a 62.4% reduction in acid value while preserving the fatty acid profile of the oil. After refining, E-field treatment was successful in removing the spent nano-adsorbent from solution (up to 72.3% by weight), demonstrating enhanced efficiency compared to conventional methods (e.g., gravitational settling, filtration, and centrifugation). The neutral oil loss using Al2O3 nano-adsorbents was also comparable to conventional refining methods, with a 4.38% (by weight) loss. After E-field treatment, the Al2O3 nano-adsorbent was then calcined to assess reusability. The Al2O3 nano-adsorbent was effectively recycled for three refining cycles. the methods do not use of large amounts of water and generate minimal waste byproducts (e.g., effluent). Nonetheless, while the nano-adsorbents demonstrated promising results in FFA removal, they were less effective in eliminating peroxides and pigments. E-field techniques were also effective in removing spent nano-adsorbent; although, optimization of E-field parameters could further improve its binding capacity. Finally, future studies could potentially focus on the physicochemical modifications of the nano-adsorbent material to enhance their refining capacity and reusability. Overall, this study presents a sustainable alternative or addition to conventional refining methods and lays the groundwork for future research. Full article
(This article belongs to the Section Food Engineering and Technology)
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28 pages, 4087 KiB  
Review
Advanced Processing Techniques and Impurity Management for High-Purity Quartz in Diverse Industrial Applications
by Hailin Long, Deqing Zhu, Jian Pan, Siwei Li, Congcong Yang and Zhengqi Guo
Minerals 2024, 14(6), 571; https://doi.org/10.3390/min14060571 - 30 May 2024
Cited by 14 | Viewed by 8199
Abstract
While numerous studies have explored the mineralogical characteristics and purification techniques of high-purity quartz (HPQ), discussions on impurity control during various purification processes and their applications in photovoltaics, electronics, and optics remain limited. This review delves into the adverse effects of impurities such [...] Read more.
While numerous studies have explored the mineralogical characteristics and purification techniques of high-purity quartz (HPQ), discussions on impurity control during various purification processes and their applications in photovoltaics, electronics, and optics remain limited. This review delves into the adverse effects of impurities such as aluminum, iron, and sodium in the manufacturing processes of these industries, emphasizing their critical role as these impurities can degrade material performance. This paper focuses on analyzing the types of impurities found in quartz and evaluates existing purification technologies such as acid washing, ultrasonic acid washing, chlorination roasting, and calcination quenching. It highlights the limitations of current technologies in processing quartz ore and discusses the advantages of different impurity types under various technological treatments. Moreover, it explores the environmental and economic impacts of these high-purity processes, underlining the necessity for more environmentally friendly and cost-effective purification techniques. The purpose of this review is to provide a comprehensive technical and strategic framework for the use of high-purity quartz in high-tech applications, supporting future research and industrial applications in this critical material field. Full article
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18 pages, 1370 KiB  
Review
An Overview of Hydrothermally Synthesized Titanate Nanotubes: The Factors Affecting Preparation and Their Promising Pharmaceutical Applications
by Ranim Saker, Hadi Shammout, Géza Regdon and Tamás Sovány
Pharmaceutics 2024, 16(5), 635; https://doi.org/10.3390/pharmaceutics16050635 - 9 May 2024
Cited by 8 | Viewed by 1884
Abstract
Recently, titanate nanotubes (TNTs) have been receiving more attention and becoming an attractive candidate for use in several disciplines. With their promising results and outstanding performance, they bring added value to any field using them, such as green chemistry, engineering, and medicine. Their [...] Read more.
Recently, titanate nanotubes (TNTs) have been receiving more attention and becoming an attractive candidate for use in several disciplines. With their promising results and outstanding performance, they bring added value to any field using them, such as green chemistry, engineering, and medicine. Their good biocompatibility, high resistance, and special physicochemical properties also provide a wide spectrum of advantages that could be of crucial importance for investment in different platforms, especially medical and pharmaceutical ones. Hydrothermal treatment is one of the most popular methods for TNT preparation because it is a simple, cost-effective, and environmentally friendly water-based procedure. It is also considered as a strong candidate for large-scale production intended for biomedical application because of its high yield and the special properties of the resulting nanotubes, especially their small diameters, which are more appropriate for drug delivery and long circulation. TNTs’ properties highly differ according to the preparation conditions, which would later affect their subsequent application field. The aim of this review is to discuss the factors that could possibly affect their synthesis and determine the transformations that could happen according to the variation of factors. To fulfil this aim, relevant scientific databases (Web of Science, Scopus, PubMed, etc.) were searched using the keywords titanate nanotubes, hydrothermal treatment, synthesis, temperature, time, alkaline medium, post treatment, acid washing, calcination, pharmaceutical applications, drug delivery, etc. The articles discussing TNTs preparation by hydrothermal synthesis were selected, and papers discussing other preparation methods were excluded; then, the results were evaluated based on a careful reading of the selected articles. This investigation and comprehensive review of different parameters could be the answer to several problems concerning establishing a producible method of TNTs production, and it might also help to optimize their characteristics and then extend their application limits to further domains that are not yet totally revealed, especially the pharmaceutical industry and drug delivery. Full article
(This article belongs to the Special Issue Advanced Pharmaceutical Excipients Used in Solid Dosage Forms)
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14 pages, 7477 KiB  
Article
Sporopollenin Capsules as Biomimetic Templates for the Synthesis of Hydroxyapatite and β-TCP
by Arianna De Mori, Daniel Quizon, Hannah Dalton, Berzah Yavuzyegit, Guido Cerri, Milan Antonijevic and Marta Roldo
Biomimetics 2024, 9(3), 159; https://doi.org/10.3390/biomimetics9030159 - 4 Mar 2024
Cited by 4 | Viewed by 3296
Abstract
Pollen grains, with their resilient sporopollenin exine and defined morphologies, have been explored as bio-templates for the synthesis of calcium phosphate minerals, particularly hydroxyapatite (HAp) and β-tricalcium phosphate (TCP). Various pollen morphologies from different plant species (black alder, dandelion, lamb’s quarters, ragweed, and [...] Read more.
Pollen grains, with their resilient sporopollenin exine and defined morphologies, have been explored as bio-templates for the synthesis of calcium phosphate minerals, particularly hydroxyapatite (HAp) and β-tricalcium phosphate (TCP). Various pollen morphologies from different plant species (black alder, dandelion, lamb’s quarters, ragweed, and stargazer lily) were evaluated. Pollen grains underwent acid washing to remove allergenic material and facilitate subsequent calcification. Ragweed and lamb’s quarter pollen grains were chosen as templates for calcium phosphate salts deposition due to their distinct morphologies. The calcification process yielded well-defined spherical hollow particles. The washing step, intended to reduce the protein content, did not significantly affect the final product; thus, justifying the removal of this low-yield step from the synthesis process. Characterisation techniques, including X-ray diffraction, scanning electron microscopy, Fourier-transform infrared spectroscopy, and thermal gravimetric analysis, confirmed the successful calcification of pollen-derived materials, revealing that calcified grains were principally composed of calcium deficient HAp. After calcination, biphasic calcium phosphate composed of HAp and TPC was obtained. This study demonstrated the feasibility of using pollen grains as green and sustainable bio-templates for synthesizing biomaterials with controlled morphology, showcasing their potential in biomedical applications such as drug delivery and bone regeneration. Full article
(This article belongs to the Section Biomimetics of Materials and Structures)
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13 pages, 3891 KiB  
Article
Performance Improvement and Microstructure Characterization of Cement-Stabilized Roadbase Materials Containing Phosphogypsum/Recycled Concrete Aggregate
by Yang Wu, Xiaoya Bian, Jie Liu, Ruan Chi and Xuyong Chen
Materials 2023, 16(19), 6607; https://doi.org/10.3390/ma16196607 - 9 Oct 2023
Cited by 8 | Viewed by 1602
Abstract
The proper reutilization of the phosphogypsum (PG) by-product derived from the production of phosphoric acid and recycled concrete aggregate (RCA) from waste concrete in roadbase materials is of great necessity and importance. This investigation tried seeking a new approach to reuse them to [...] Read more.
The proper reutilization of the phosphogypsum (PG) by-product derived from the production of phosphoric acid and recycled concrete aggregate (RCA) from waste concrete in roadbase materials is of great necessity and importance. This investigation tried seeking a new approach to reuse them to high quality, including turning PG into calcinated PG (CPG) via washing and calcination, as well as adopting sodium metasilicate nonahydrate (SMN) to strengthen the roadbase materials of cement-stabilized CPG and RCA. Upon the mix design, with a series of experiments including unconfined compressive strength, the wet–dry cycle, freeze–thaw cycle, and scanning electron microscopy, the comprehensive effects of PG treatment, the CPG to RCA mix ratio, SMN dosage, wet–dry cycle and freeze–thaw cycle on the road performance of roadbase materials were well evaluated, and the traffic bearing capacity and microstructure characteristics were also analyzed. The results demonstrate that the 7 d unconfined compressive strength of CPG/RCA roadbase materials can reach 5.34 MPa as the CPG and SMN dosage are 20% and 11%, respectively, which meets the requirements of an extremely and very heavy traffic grade. After five wet–dry cycles and freeze–thaw cycles, the resistance of the CPG/RCA roadbase materials to moisture and frost was significantly improved as 11% SMN was added. Meanwhile, SMN contributes to the reduction in crack width and densifies the microstructure of CPG/RCA roadbase materials. The research results can be used to provide new guidance for building more durable roadbase materials. Full article
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15 pages, 5310 KiB  
Article
Assessment of the Stabilization of Cu-, Pb-, and Zn-Contaminated Fine Soil Using Cockle Shells, Scallop Shells, and Starfish
by Sang Hyeop Park, Jinsung An, Agamemnon Koutsospyros and Deok Hyun Moon
Agriculture 2023, 13(7), 1414; https://doi.org/10.3390/agriculture13071414 - 17 Jul 2023
Cited by 9 | Viewed by 2195
Abstract
Soil washing is a well-established remediation technology for treating soil contaminated with heavy metals. It involves the separation of contaminants from the soil using acidic washing agents. Nevertheless, the application of washing agents at high concentrations may lead to soil acidification and the [...] Read more.
Soil washing is a well-established remediation technology for treating soil contaminated with heavy metals. It involves the separation of contaminants from the soil using acidic washing agents. Nevertheless, the application of washing agents at high concentrations may lead to soil acidification and the destruction of the clay structure. To avert this problem, recently, a soil washing variant has been presented, which solely employs high-pressure water without any chemical solvents. However, the fine soil generated from soil washing at a high-pressure contains high levels of heavy metals and requires proper treatment. This study examines the use and applicability of natural aquaculture materials as stabilizing agents for treating heavy metals (Cu, Pb, and Zn) in fine soil generated by high-pressure soil washing. Three aquaculture materials were assessed, namely, cockle shells (CKS), scallop shells (SLS), and Asterias amurensis starfish (ASF). Each material was processed to yield three types of stabilizing agents: natural type (-#10 mesh), natural type (-#20 mesh), and calcined(C) type (-#10 mesh). Each stabilizing agent was added to the contaminated soil at a ratio of 0 to 10 wt%, and then, mixed with an appropriate amount of water. After wet curing for 28 days, the stabilization efficiency of Cu, Pb, and Zn was evaluated using 0.1 N HCl solution. The elution of heavy metals showed a decreasing trend with higher dosages of stabilizing agents. The calcined type (-#10) showed the highest stabilization efficiency, followed by the natural type (-#20) and natural type (-#10). In addition, a comparison of the efficiency of the different stabilizing agents showed that calcined ASF (CASF) had the highest stabilization efficiency, followed by calcined SLS (CSLS), calcined CKS (CCKS), natural ASF (NASF), natural SLS (NSLS), and natural CKS. Finally, analysis of samples exhibiting the highest stabilization efficiency by scanning electron microscopy–energy dispersive X-ray spectrometry (SEM–EDX) confirmed that the pozzolanic reaction contributed to the stabilization treatment. The results of this study demonstrate that heavy metal-contaminated fine soil, generated by high-pressure washing, can be remediated by stabilizing Cu, Pb, and Zn using waste aquaculture materials (CKS, SLS, and ASF), which are often illegally dumped into the sea or landfills and cause environmental damage. Full article
(This article belongs to the Section Agricultural Soils)
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19 pages, 5204 KiB  
Article
Deep Processing of Dump Slag from the Copper-Nickel Industry
by Alexandr G. Kasikov, Elena A. Shchelokova, Olga A. Timoshchik and Vasilij V. Semushin
Metals 2023, 13(7), 1265; https://doi.org/10.3390/met13071265 - 13 Jul 2023
Cited by 6 | Viewed by 2212
Abstract
This work proposes an environmentally safe and economically feasible method of waste copper-nickel production slag utilization (Kola Mining-Metallurgical Company, Nornickel, Kola Peninsula, Russia). This process involves the decomposition of slag by diluted solutions of sulfuric acid (7–10 wt.% H2SO4) [...] Read more.
This work proposes an environmentally safe and economically feasible method of waste copper-nickel production slag utilization (Kola Mining-Metallurgical Company, Nornickel, Kola Peninsula, Russia). This process involves the decomposition of slag by diluted solutions of sulfuric acid (7–10 wt.% H2SO4) with a transfer in a solution of more than 70% silicon, 77% iron and 78% magnesium, and a concentration of non-ferrous metals in the residue (~70%). Copper ions were used in the leaching stage to prevent the release of hydrogen sulfide into the working atmosphere. Dehydration of the solution, followed by washing of water-soluble sulphates from silica, was carried out to separate silica from the leaching solution. The dehydration temperature effect on the silica structural characteristics was determined. The possibility of recovering non-ferrous metals from solutions after silica extraction by precipitation, in the form of copper cementite, and the sum of nickel and cobalt sulfides, was evaluated. Pigment-grade iron dioxide, magnesium sulphate and aluminium hydroxide were obtained by dehydration of the solution after extraction of base metals, calcination and other operations. Sulfuric acid leaching resulted in the disclosure of sulfide grains encapsulated in ferrosilicate, which is a favorable factor for flotation. The depleted residue can be successfully used in the construction industry. Full article
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14 pages, 4771 KiB  
Article
Investigation on the Value-Added Production of Silicon Dioxide and Synthesizing Zeolites as well as Extraction of Rare Earth Elements from Fly Ash
by Zhe Sun, Heyu Li, Zuimiao Tao, Baochuan Wang, Lei Gao, Yusheng Xu and Yan Cao
Appl. Sci. 2023, 13(12), 7250; https://doi.org/10.3390/app13127250 - 17 Jun 2023
Cited by 1 | Viewed by 1924
Abstract
Coal fly ash is one of the most promising secondary sources for extracting high value-added rare earth elements. Nevertheless, the majority of rare earth elements in coal fly ash are associated with the aluminosilicate glassy phase, hindering their solubility during the acid leaching [...] Read more.
Coal fly ash is one of the most promising secondary sources for extracting high value-added rare earth elements. Nevertheless, the majority of rare earth elements in coal fly ash are associated with the aluminosilicate glassy phase, hindering their solubility during the acid leaching process and resulting in the traditional rare earth elements extraction method, which is unavoidably complex in operation and poor in the economy. In this study, prior to the conventional acid leaching, the realization of the coal fly ash activation was considered. This consisted of two steps involving the coal fly ash calcination at the elevated temperatures using recyclable Na2CO3 and the water and alkali washing. It helped in developing the pore structures in coal fly ash, facilitating the leaching solution to rare earth elements, and reducing the acid consumption of rare earth elements leaching. Simultaneously, the generated aqueous solutions could precipitate two new valuable products, the purified silica oxide powder (257.58 g·kg−1, 338.1 m2·g−1 BET, 40 nm grain size, 93.43% purity) and porous zeolites (410.3 g·kg−1). The residual rare earth elements in the pretreated solid residue can be easily extracted, with an extraction efficiency of 91.24% and an acid saving rate of 74.5%. Therefore, a multiple of value-added products can be obtained by this new extraction method with great economic significance. Full article
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20 pages, 6196 KiB  
Article
Monodispersed NiO Nanoparticles into SBA-15: An Efficient Nanocatalyst to Produce Ketone-Alcohol (KA) Oil by the Oxidation of Cyclohexane in Mild Conditions
by Mohamed Abboud, Reem S. Alnefaie, Asla A. AL-Zahrani, Nabil Al-Zaqri, Mohammad Abu Haija, Azza Al-Ghamdi, Mabkhoot Alsaiari, Mohammed Jalalah, Omeer Albormani and Mohamed S. Hamdy
Sustainability 2023, 15(7), 5817; https://doi.org/10.3390/su15075817 - 27 Mar 2023
Cited by 2 | Viewed by 2224
Abstract
A simple and efficient approach to preparing highly efficient and reusable NiO@SBA-15 nanocatalysts for the oxidation of cyclohexane to produce ketone-alcohol (KA) oil was reported. These nanocatalysts were prepared by the dispersion of NiO NPs into SBA-15 using a coordination-assisted grafting method. In [...] Read more.
A simple and efficient approach to preparing highly efficient and reusable NiO@SBA-15 nanocatalysts for the oxidation of cyclohexane to produce ketone-alcohol (KA) oil was reported. These nanocatalysts were prepared by the dispersion of NiO NPs into SBA-15 using a coordination-assisted grafting method. In this approach, four commercially available nickel salts were immobilized into amino-functionalized SBA-15. After washing and calcination, four new nanocatalysts were obtained. The high dispersion of NiO NPs into SBA-15 was confirmed by HR-TEM and XRD. Different oxidants such as O2, H2O2, t-butyl hydrogen peroxide (TBHP), and meta-Chloroperoxybenzoic acid (m-CPBA) were evaluated. However, m-CPBA exhibited the highest catalytic activity. Compared to different catalysts reported in the literature, for the first time, 75–99% of cyclohexane was converted to KA oil over NiO@SBA-15. In addition, the cyclohexane conversion and K/A ratio were affected by the reaction time, catalyst dose, Ni content, and NiO dispersion. Moreover, NiO@SBA-15 maintained a high catalytic activity during five successive cycles. Full article
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15 pages, 3850 KiB  
Article
Effect of Carbonization Temperature of Rice Husk Char Preparation on SiC Structure and Composition of By-Products in SiC Synthesis with Magnesiothermic Reduction Method
by Solihudin Solihudin, Haryono Haryono, Atiek Rostika Noviyanti and Akrajas Ali Umar
Processes 2023, 11(1), 133; https://doi.org/10.3390/pr11010133 - 2 Jan 2023
Cited by 1 | Viewed by 1938
Abstract
The structure of rice husk char is one of the factors that influence the morphology of SiC and the composition of by-products in the magnesiothermic reduction. This structure can be improved by carbonization. Therefore, this study aims to examine the effect of the [...] Read more.
The structure of rice husk char is one of the factors that influence the morphology of SiC and the composition of by-products in the magnesiothermic reduction. This structure can be improved by carbonization. Therefore, this study aims to examine the effect of the carbonization temperature of rice husk char on the structure of SiC and identify the by-products formed by the magnesiothermic reduction. The rice husk char was made by carbonization at various temperatures of 700, 800, 900, and 1000 °C. They were converted to SiC by magnesiothermic reduction at 600 °C, washing with hydrochloric acid, calcination at 700 °C in an air atmosphere, and washing with a mixture of hydrofluoric acid and acetic acid. The products were characterized by FT-IR, XRD, and SEM-EDS. The results showed that creating SiC using the magnesiothermic method with carbonization at a temperature of 1000 °C produced a polytype 2H-SiC, and the by-products were MgO, Mg2SiO4, and Si. MgO was successfully separated in the washing step with a hydrochloric acid solution, while Mg2SiO4 was separated from SiC by washing using a mixture of hydrofluoric acid and acetic acid. Full article
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23 pages, 3869 KiB  
Article
Aqueous-Phase Glycerol Conversion over Ni-Based Catalysts Synthesized by Nanocasting
by Adriana Morales-Marín, Unai Iriarte-Velasco, Miguel Ángel Gutiérrez-Ortiz and Jose Luis Ayastuy
Catalysts 2022, 12(6), 668; https://doi.org/10.3390/catal12060668 - 18 Jun 2022
Cited by 2 | Viewed by 2552
Abstract
A morphological strategy consisting of nanocasting synthesis of nickel aluminate spinel precursor was addressed. Two nanocasted catalysts were synthesized involving different template-removal procedures (i.e., Teflon-assisted calcination vs. NaOH washing) for spinel recovery. As a reference, spinel NiAl2O4 supported by SBA-15 [...] Read more.
A morphological strategy consisting of nanocasting synthesis of nickel aluminate spinel precursor was addressed. Two nanocasted catalysts were synthesized involving different template-removal procedures (i.e., Teflon-assisted calcination vs. NaOH washing) for spinel recovery. As a reference, spinel NiAl2O4 supported by SBA-15 and bare nickel aluminate spinel were selected. The obtained solids were characterized in detail, examining their textural, acid–base, structural and compositional characteristics, either in the calcined or reduced forms. The as-obtained catalysts’ performance was evaluated in the aqueous-phase reforming of glycerol at 235 °C and 35 bar. Exhausted samples were also characterized to enlighten changes in catalyst properties during the aqueous-phase reaction. NiAl/SBA-15 and NiAl-NCF catalyst showed very poor catalytic performance for the glycerol transformation. NiAl-NCN catalyst presented improved activity with respect to NiAl, with a 20% higher hydrogen production rate but, as a drawback, higher methane formation for a whole range of glycerol conversions. Exhausted catalyst indicated nickel oxidized in liquid phase reaction. Full article
(This article belongs to the Special Issue Catalytic Conversion of Glycerol)
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13 pages, 3821 KiB  
Article
Wasteless Synthesis and Properties of Highly Dispersed MgAl2O4 Based on Product of Thermal Activation of Gibbsite
by Aleksey V. Zhuzhgov, Vasily Y. Kruglyakov, Tatyana S. Glazneva, Evgeny A. Suprun and Lyubov A. Isupova
Chemistry 2022, 4(2), 316-328; https://doi.org/10.3390/chemistry4020024 - 11 Apr 2022
Cited by 3 | Viewed by 2565
Abstract
The study showed that the interaction of the product of centrifugal thermal activation of gibbsite with an aqueous solution of magnesium nitrate at a cationic ratio Mg:Al = 1:2 leads to the formation of mixed double hydroxides both under hydrothermal treatment at 150 [...] Read more.
The study showed that the interaction of the product of centrifugal thermal activation of gibbsite with an aqueous solution of magnesium nitrate at a cationic ratio Mg:Al = 1:2 leads to the formation of mixed double hydroxides both under hydrothermal treatment at 150 °C and at room temperature. The subsequent thermal treatment at 550 °C of the product of mild interaction leads to ~90% alumina-magnesia spinel and ~10% MgO, while the treatment of the hydrothermal interaction product leads to ~100% spinel with the stoichiometric composition MgAl2O4. The obtained spinel samples possess a high specific surface area (above 100 m2/g) and a hierarchical pore structure formed by the micron-level particles of different sizes (1–2 and 10–20 μm) consisting of ~70 nm crystallites with ~3 nm pores; the samples differ mostly in the total volume and quantitative ratio of the pores. The samples have Lewis acid sites of moderate strength on the surface, the amount of which is much lower to how it is when compared with a sample prepared by precipitation in that they also differ by quantity from each other as well (503 μmol/g for stoichiometric spinel and 304 μmol/g for sample with admixture of MgO). As the calcination temperature is raised to 850 °C, the acidity decreases—only weak Lewis acid sites are observed, the amount of which is also higher for stoichiometric spinel (161 and 39 μmol/g, respectively). The method proposed for the synthesis of alumina-magnesia systems provides a high dispersion and a much lower surface acidity for the oxides; in addition, it minimizes or completely excludes wash water, in distinction to the precipitation method. Full article
(This article belongs to the Special Issue Earth-Abundant Metal Chemistry and Catalysis)
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