scholarly journals Synthesis and characterization of Na-P1 (GIS) zeolite using a kaolinitic rock

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Daniela Novembre ◽  
Domingo Gimeno ◽  
Alessandro Del Vecchio

AbstractThis work focuses on the hydrothermal synthesis of Na-P1 zeolite by using a kaolinite rock coming from Romana (Sassari, Italy). The kaolin is calcined at a temperature of 650 °C and then mixed with calculated quantities of NaOH. The synthesis runs are carried out at ambient pressure and at variable temperatures of 65 and 100 °C. For the first time compared to the past, the Na-P1 zeolite is synthesized without the use of additives and through a protocol that reduces both temperatures and synthesis times. The synthesis products are analysed by X-ray diffraction, high temperature X-ray diffraction, infrared spectroscopy, scanning electron microscopy and inductively coupled plasma optical emission spectrometry. The cell parameters are calculated using the Rietveld method. Density and specific surface area are also calculated. The absence of amorphous phases and impurities in synthetic powders is verified through quantitative phase analysis using the combined Rietveld and reference intensity ratio methods. The results make the experimental protocol very promising for an industrial transfer.

2020 ◽  
Author(s):  
Daniela Novembre ◽  
Domingo Gimeno ◽  
Alessandro Del Vecchio

Abstract This work focuses on the hydrothermal synthesis of Na-P1 zeolite by using a kaolinite rock coming from Romana (Sassari, Italy). The kaolin is calcined at a temperature of 650 °C and then mixed with calculated quantities of NaOH. The synthesis runs are carried out at ambient pressure and at variable temperatures of 65 ° and 100 °C. For the first time compared to the past, the Na-P1 zeolite is synthesized without the use of additives and through a protocol that reduces both temperatures and synthesis times. The synthesis products are analysed by X-ray diffraction, high temperature X-ray diffraction, infrared spectroscopy, scanning electron microscopy and inductively coupled plasma optical emission spectrometry. The cell parameters are calculated using the Rietveld method. Density and specific surface area are also calculated. The absence of amorphous phases and impurities in synthetic powders is verified through quantitative phase analysis using the combined Rietveld and reference intensity ratio methods.The results make the experimental protocol very promising for an industrial transfer.


2018 ◽  
Vol 82 (4) ◽  
pp. 961-973 ◽  
Author(s):  
Daniela Novembre ◽  
Domingo Gimeno ◽  
Nicola d'Alessandro ◽  
Lucia Tonucci

ABSTRACTThe present work deals with the synthesis of kalsilite using material from a kaolinitic rock outcrop in Romana, Sassary Province, Sardinia, Italy.The hydrothermal synthesis method required the dissolution of kaolin and Al(OH)3 in a KOH solution at a temperature of 190°C and 1.013 bar. Crystallization of kalsilite was confirmed at 12 h in association with kaliophilite H2 as a metastable phase.The products of synthesis were fully characterized by powder X-ray diffraction, scanning electron microscopy, inductively coupled plasma optical emission spectrometry, infrared spectroscopy and 29Si nuclear magnetic resonance. The amorphous phase in the synthesis powders was estimated with quantitative phase analysis using the combined Rietveld and reference intensity ratio methods. Cell parameters and density were also calculated for the kalsilite. A potential application of kalsilite was investigated as a heterogeneous catalyst for biodiesel synthesis from sunflower oil used for frying.


Materials ◽  
2021 ◽  
Vol 14 (13) ◽  
pp. 3680
Author(s):  
Bo Li ◽  
Yaowu Wang ◽  
Bingliang Gao

A selective liquation process to extract Al from a coarse Al–Si alloy, produced by carbothermal reduction, was investigated on the laboratory scale. The products obtained by selective liquation–vacuum distillation were analyzed by X-ray diffraction, inductively coupled plasma optical emission spectrometry and scanning electron microscopy. During the selective liquation process with the use of zinc as the solvent, the pure aluminum in the coarse Al–Si alloy dissolved in the zinc melt to form an α-solid solution with zinc, and most of the silicon and iron-rich phases and Al–Si–Fe intermetallics precipitated and grew into massive grains that entered into the slag and separated with the Zn–Al alloy melt. However, some fine silicon particles remained in the Zn–Al alloy. Thus, Al–Si alloys conforming to industrial application standards were obtained when the Zn–Al alloys were separated by a distillation process.


2020 ◽  
Vol 9 (1) ◽  
pp. 1586-1593
Author(s):  
Tingting Yan ◽  
Shengwen Zhong ◽  
Miaomiao Zhou ◽  
Xiaoming Guo ◽  
Jingwei Hu ◽  
...  

Abstract The extraction of Li from the spent LiFePO4 cathode is enhanced by the selective removal using interactions between HCl and NaClO to dissolve the Li+ ion while Fe and P are retained in the structure. Several parameters, including the effects of dosage and drop acceleration of HCl and NaClO, reaction time, reaction temperature, and solid–liquid ratio on lithium leaching, were tested. The Total yields of lithium can achieve 97% after extraction process that lithium is extracted from the precipitated mother liquor, using an appropriate extraction agent that is a mixture of P507 and TBP and NF. The method also significantly reduced the use of acid and alkali, and the economic benefit of recycling is improved. Changes in composition, morphology, and structure of the material in the dissolution process are characterized by inductively coupled plasma optical emission spectrometry, scanning electron microscope, X-ray diffraction, particle size distribution instrument, and moisture analysis.


Materials ◽  
2019 ◽  
Vol 12 (19) ◽  
pp. 3267
Author(s):  
Gigliola Lusvardi ◽  
Francesca Sgarbi Stabellini ◽  
Roberta Salvatori

(1) Background: valuation of the bioactivity and cytocompatibility of P2O5-free and CeO2 doped glasses. (2) Methods: all glasses are based on the Kokubo (K) composition and prepared by a melting method. Doped glassed, K1.2, K3.6 and K5.3 contain 1.2, 3.6, and 5.3 mol% of CeO2. Bioactivity and cytotoxicity tests were carried out in simulated body fluid (SBF) solution and murine osteocyte (MLO-Y4) cell lines, respectively. Leaching of ions concentration in SBF was determined by inductively coupled plasma mass spectrometry (ICP-MS) and optical emission spectrometry (ICP-OES). The surface of the glasses were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) techniques. (3) Results: P2O5-free cerium doped glasses are proactive according to European directives. Cerium increases durability and retards, but does not inhibit, (Ca10(PO4)6(OH)2, HA) formation at higher cerium amounts (K3.6 and K5.3); however, cell proliferation increases with the amount of cerium especially evident for K5.3. (4) Conclusions: These results enforce the use of P2O5-free cerium doped bioactive glasses as a new class of biomaterials.


2015 ◽  
Vol 6 ◽  
pp. 1957-1969 ◽  
Author(s):  
Jacek Wojnarowicz ◽  
Sylwia Kusnieruk ◽  
Tadeusz Chudoba ◽  
Stanislaw Gierlotka ◽  
Witold Lojkowski ◽  
...  

Zinc oxide nanopowders doped with 1–15 mol % cobalt were produced by the microwave solvothermal synthesis (MSS) technique. The obtained nanoparticles were annealed at 800 °C in nitrogen (99.999%) and in synthetic air. The material nanostructure was investigated by means of the following techniques: X-ray diffraction (XRD), helium pycnometry density, specific surface area (SSA), inductively coupled plasma optical emission spectrometry (ICP-OES), extended X-ray absorption fine structure (EXAFS) spectroscopy, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and with magnetometry using superconducting quantum interference device (SQUID). Irrespective of the Co content, nanoparticles in their initial state present a similar morphology. They are composed of loosely agglomerated spherical particles with wurtzite-type crystal structure with crystallites of a mean size of 30 nm. Annealing to temperatures of up to 800 °C induced the growth of crystallites up to a maximum of 2 μm in diameter. For samples annealed in high purity nitrogen, the precipitation of metallic α-Co was detected for a Co content of 5 mol % or more. For samples annealed in synthetic air, no change of phase structure was detected, except for precipitation of Co3O4 for a Co content of 15 mol %. The results of the magentometry investigation indicated that all as-synthesized samples displayed paramagnetic properties with a contribution of anti-ferromagnetic coupling of Co–Co pairs. After annealing in synthetic air, the samples remained paramagnetic and samples annealed under nitrogen flow showed a magnetic response under the influences of a magnetic field, likely related to the precipitation of metallic Co in nanoparticles.


Coatings ◽  
2020 ◽  
Vol 10 (6) ◽  
pp. 553
Author(s):  
Dominik Höhlich ◽  
Thomas Mehner ◽  
Ingolf Scharf ◽  
Thomas Lampke

Ag–W two-phase system was prepared by electrodeposition using anhydrous 1-ethyl-3-methylimidazolium chloride [EMIm]Cl ionic-liquid (IL) solution with AlCl3 in different ratios. The deposition took place outside the glove box with a continuous Ar stream over the electrolyte at 120 °C and a pulsed-like current regime. Resultant layers show areas of Ag and W with an overall W content with a mass fraction of w W   = 50% (mole fraction x W   = 36.9%). The phase composition of Ag–W layers was observed by X-ray diffraction, and the chemical composition was characterized by scanning electron microscopy and inductively coupled plasma optical emission spectroscopy.


Minerals ◽  
2018 ◽  
Vol 8 (10) ◽  
pp. 465 ◽  
Author(s):  
Roberto da Conceição Ribeiro ◽  
Patrícia Marques Ferreira de Figueiredo ◽  
Daniel Silva Barbutti

Master Valentim’s fountain has become an important historical patrimony for Brazil, being portrayed by famous artists, among them Jean-Baptiste Debret. In 1938, it was registered as cultural heritage by the Brazilian National Historical and Artistic Heritage Institute (IPHAN), and in 1990 it was subjected to excavation and restoration works. The fountain was built in Gneiss and Lioz limestone, with metallic plates and mortar connecting the Gneiss blocks. Currently, deteriorations in the fountain stones can be observed, such as light stains and some aesthetic modifications caused by inadequate restorations. Petrography, X-ray fluorescence (XRF), XRD, physical properties, colorimetry, electrical conductivity, inductively coupled plasma optical emission spectrometry (ICP-OES), scanning electron microscopy-energy dispersive X-ray (SEM-EDX), and TGA were performed in order to characterize the Gneiss blocks, the metallic plates, and the stones used in previous restorations, as well as light stains observed on the Gneiss blocks. The petrography and XRD analyses inferred that the light stains may have been caused by the formation of an insoluble salt as a result of the association of the lead from the plates with other elements. The XRD analysis on the light staining area indicated the presence of cerussite (PbCO3) and anglesite (PbSO4), which are the probable cause of the light stains. The SEM-EDX results suggested that sulfur is the main element associated to lead.


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