scholarly journals KINETICS ASPECT OF HYDROCHEMICAL FLUORINATION OF SILICON-CONTAINING INDUSTRIAL WASTE

2021 ◽  
pp. 900-909
Author(s):  
Ирина Сергеевна Медянкина ◽  
Владимир Михайлович Скачков ◽  
Лилия Александровна Пасечник
Keyword(s):  
Particle Size ◽  
Kinetic Equation ◽  
Amorphous Silica ◽  
Industrial Waste ◽  
Sol Gel ◽  
Average Density ◽  
Ammonium Hexafluorosilicate ◽  
Developed Surface ◽  
Silicon Solubility ◽  
Titanium Vanadium

Предложен способ получения высокодисперсного аморфного кремнезема из отходов обогащения низкотитанистых ванадий содержащих титаномагнетитов АО «ЕВРАЗ Качканарский ГОК» - хвостов мокрой магнитной сепарации. Применение раствора гидрофторида аммония ( NHHF) позволяет практически селективно извлечь кремний в раствор в виде гексафторосиликата аммония. Степень извлечения кремния раствором 1,0 - 2,5 мас.% NHHF за 6 часов составляет 46%. Диффузионный процесс выщелачивания кремния из ХММС описывается кинетическим уравнением 1 -(1 -а) = 0,0043• exp(-5230/RT)-г . Аморфный кремнезем SiO, полученный золь- гель методом из фторидного кремнийсодержащего раствора, имеет высокоразвитую поверхность S = 320 м/г, рассчитанный из средней плотности «белой сажи» размер частиц составляет d = 10 нм. Увеличение концентрации NHHF до 20 мас.% приводит к повышению растворимости кремния, а также других компонентов хвостов мокрой магнитной сепарации, которые являются нежелательными примесями в конечном продукте SiO. В целом показана перспективность гидрохимического выщелачивания кремнийсодержащих промышленных отходов - хвостов мокрой магнитной сепарации слабыми растворами гидрофторида аммония для синтеза чистого аморфного SiO. A method for producing amorphous silica from the enrichment wastes of low-titanium vanadium containing titanomagnetites of JSC «EVRAZ ZSMK» - wet magnetic separation tailings is proposed. The use of a NHHF solution makes it possible to practically selectively extract silicon into the solution in the form of ammonium hexafluorosilicate. The extraction of silicon with 1,0 - 2,5 wt.% NHHF solution for 6 hours reached 46%. The diffusion process of the silicon extraction is described by the kinetic equation 1 - (1 - a) = 0,0043 • exp(-5230 / RT)• t . Amorphous silica obtained by the sol-gel method from a fluoride silicon-containing solution has a highly developed surface 320 m/g, the particle size calculated from the average density of «white carbon black» is of 10 nm. The increase in concentration to 20 wt. % NHHF leads to the rise of the silicon solubility and of other tailings components, which are unwanted impurities in the final product. In general, it is shown that the hydrochemical leaching of silicon-containing industrial waste - tailings with weak solutions of ammonium hydrofluoride is promising for the synthesis of pure amorphous silica.

Sol-Gel Synthesis of Amorphous Silica Nanoparticles: Study of the Process Parameters Influence on Structure and Particle Size Distribution

2018 ◽  
Vol 912 ◽  
pp. 77-81
Author(s):  
Renata Deliberato Aspasio ◽  
Jairo Freitas da Silva Jr. ◽  
Roger Borges ◽  
Juliana Marchi
Keyword(s):  
Particle Size ◽  
Particle Size Distribution ◽  
Silica Nanoparticles ◽  
Size Distribution ◽  
Functional Groups ◽  
Process Parameters ◽  
Amorphous Silica ◽  
Sol Gel ◽  
Molar Ratio ◽  
Sol Gel Synthesis

The synthesis of silica particles at the nanoscale through the sol-gel method is of great interest due to their potential use in industrial applications. The Stöber method is the most used method for the silica nanoparticles production using ammonia as a catalyst. This work studied the sol-gel synthesis of amorphous silica nanoparticles described by Stöber, in order to evaluate the influence of the variation of the process parameters (molar ratio water/TEOS = 25 and 55, reagent feed rate = 0.6 mL/min and 18 mL/min, pH = 12 and 9 and reaction time of 0, 5, 30, 60 and 120 minutes) on the particle size distribution and structural functional groups. The particle size distribution was analyzed by dynamic light scattering (DLS) and the structural functional groups was analyzed by infrared spectroscopy through Fourier transform (FTIR). The molar ratio water/TEOS influenced the functional groups presents and the time influenced the particle diameter distribution. It was not possible to identify the influence of the feed rate and pH in the results. The particle diameters found were between 200-500nm. This result may be occurred due to mass diffusion and/or nanoparticles aggregation.

scholarly journals Feasibility of fly ash as fluxing agent in mid- and low-grade phosphate rock carbothermal reduction and its reaction kinetics

2021 ◽  
Vol 10 (1) ◽  
pp. 157-168
Author(s):  
Biwei Luo ◽  
Pengfei Li ◽  
Yan Li ◽  
Jun Ji ◽  
Dongsheng He ◽  
...  
Keyword(s):  
Particle Size ◽  
Fly Ash ◽  
Reaction Time ◽  
Carbothermal Reduction ◽  
Industrial Waste ◽  
Phosphate Rock ◽  
Molar Ratio ◽  
Low Grade ◽  
Carbon Excess ◽  
Fluxing Agent

Abstract The feasibility of industrial waste fly ash as an alternative fluxing agent for silica in carbothermal reduction of medium-low-grade phosphate ore was studied in this paper. With a series of single-factor experiments, the reduction rate of phosphate rock under different reaction temperature, reaction time, particle size, carbon excess coefficient, and silicon–calcium molar ratio was investigated with silica and fly ash as fluxing agents. Higher reduction rates were obtained with fly ash fluxing instead of silica. The optimal conditions were derived as: reaction temperature 1,300°C, reaction time 75 min, particle size 48–75 µm, carbon excess coefficient 1.2, and silicon–calcium molar ratio 1.2. The optimized process condition was verified with other two different phosphate rocks and it was proved universally. The apparent kinetics analyses demonstrated that the activation energy of fly ash fluxing is reduced by 31.57 kJ/mol as compared with that of silica. The mechanism of better fluxing effect by fly ash may be ascribed to the fact that the products formed within fly ash increase the amount of liquid phase in the reaction system and promote reduction reaction. Preliminary feasibility about the recycling of industrial waste fly ash in thermal phosphoric acid industry was elucidated in the paper.

scholarly journals Sol-Gel Synthesis of the Double Perovskite Sr2FeMoO6 by Microwave Technique

Materials ◽  
2021 ◽  
Vol 14 (14) ◽  
pp. 3876
Author(s):  
Jesús Valdés ◽  
Daniel Reséndiz ◽  
Ángeles Cuán ◽  
Rufino Nava ◽  
Bertha Aguilar ◽  
...  
Keyword(s):  
Particle Size ◽  
Hydrothermal Synthesis ◽  
Microwave Radiation ◽  
Structural Characteristics ◽  
Sol Gel ◽  
Synthesis Method ◽  
Double Perovskite ◽  
Synthesis Methods ◽  
X Ray ◽  
Sol Gel Synthesis

The effect of microwave radiation on the hydrothermal synthesis of the double perovskite Sr2FeMoO6 has been studied based on a comparison of the particle size and structural characteristics of products from both methods. A temperature, pressure, and pH condition screening was performed, and the most representative results of these are herein presented and discussed. Radiation of microwaves in the hydrothermal synthesis method led to a decrease in crystallite size, which is an effect from the reaction temperature. The particle size ranged from 378 to 318 nm when pH was 4.5 and pressure was kept under 40 bars. According to X-ray diffraction (XRD) results coupled with the size-strain plot method, the product obtained by both synthesis methods (with and without microwave radiation) have similar crystal purity. The Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Spectroscopy (EDS) techniques showed that the morphology and the distribution of metal ions are uniform. The Curie temperature obtained by thermogravimetric analysis indicates that, in the presence of microwaves, the value was higher with respect to traditional synthesis from 335 K to 342.5 K. Consequently, microwave radiation enhances the diffusion and nucleation process of ionic precursors during the synthesis, which promotes a uniform heating in the reaction mixture leading to a reduction in the particle size, but keeping good crystallinity of the double perovskite. Precursor phases and the final purity of the Sr2FeMoO6 powder can be controlled via hydrothermal microwave heating on the first stages of the Sol-Gel method.

Annealing Effects on the Physical and Magnetic Properties of Tb1.5Y1.5Fe5O12 Films Nanoparticles Prepared by Sol-Gel Method

2013 ◽  
Vol 756 ◽  
pp. 91-98 ◽  
Author(s):  
Ftema W. Aldbea ◽  
Noor Bahyah Ibrahim ◽  
Mustafa Hj. Abdullah
Keyword(s):  
Particle Size ◽  
Magnetic Properties ◽  
Annealing Temperature ◽  
Quartz Substrate ◽  
Sol Gel ◽  
Lattice Parameter ◽  
Gel Method ◽  
X Ray ◽  
Sol Gel Method ◽  
Iron Garnet

Terbium –substituted yttrium iron garnet (Tb1.5Y1.5Fe5O12) films nanoparticles were successfully prepared by a sol-gel method. The films were deposited on the quartz substrate using spin coating technique. To study effect of annealing temperature, the annealing process was executed at 700, 800 and 900 °C in air for 2 hours. The X-ray diffraction (XRD) proved that the pure phase of garnet structure was detected for the film annealed at 900 °C. The lattice parameter increased with the increment of annealing temperature and the highest value of 12.35 Å was obtained at 900 °C. Field Emission Scanning Electron Microscope (FE-SEM) results showed that the particle size increased from 43nm to 56nm as annealing temperature increased from 700 to 900°C. The film’s thickness also affected by increasing of annealing temperature and become thin at 900 °C due to densification process occurred at high annealing temperature. The elemental compositions of the Tb1.5Y1.5Fe5O12 film were detected using an Energy Dispersive X-raySpectroscopy (EDX). Magnetic properties at room temperature were measured using a Vibrating Sample Magnetometer (VSM).The saturation magnetization Ms increased with the annealingtemperature and showed a high value of 104emu/cm3, but the coercivity Hc of the film was decreased due to the increment of the particle size. Normal 0 21 false false false MS X-NONE X-NONE MicrosoftInternetExplorer4 Terbium –substituted yttrium iron garnet (Tb1.5Y1.5Fe5O12) films nanoparticles were successfully prepared by a sol-gel method. The films were deposited on the quartz substrate using spin coating technique. To study effect of annealing temperature, the annealing process was executed at 700, 800 and 900°C in air for 2 hours. The X-ray diffraction (XRD) proved that the pure phase of garnet structure was detected for the film annealed at 900 °C. The lattice parameter increased with the increment of annealing temperature and the highest value of 12.35 Å was obtained at 900 °C. Field Emission Scanning Electron Microscope (FE-SEM) results showed that the particle size increased from 43nm to 56nm as annealing temperature increased from 700 to 900 °C. The film’s thickness also affected by increasing of annealing temperature and become thin at 900 °C due to densification process occurred at high annealing temperature. The elemental compositions of the Tb1.5Y1.5Fe5O12 film were detected using an Energy Dispersive X-ray Spectroscopy (EDX). Magnetic properties at room temperature were measured using a Vibrating Sample Magnetometer (VSM).The saturation magnetization Ms increased with the annealing temperature and showed a high value of 104emu/cm3, but the coercivity Hc of the film was decreased due to the increment of the particle size. st1\:*{behavior:url(#ieooui) } /* Style Definitions */ table.MsoNormalTable {mso-style-name:"Table Normal"; mso-tstyle-rowband-size:0; mso-tstyle-colband-size:0; mso-style-noshow:yes; mso-style-priority:99; mso-style-qformat:yes; mso-style-parent:""; mso-padding-alt:0cm 5.4pt 0cm 5.4pt; mso-para-margin:0cm; mso-para-margin-bottom:.0001pt; mso-pagination:widow-orphan; font-size:11.0pt; font-family:"Calibri","sans-serif"; mso-ascii-font-family:Calibri; mso-ascii-theme-font:minor-latin; mso-fareast-font-family:"Times New Roman"; mso-fareast-theme-font:minor-fareast; mso-hansi-font-family:Calibri; mso-hansi-theme-font:minor-latin; mso-bidi-font-family:"Times New Roman"; mso-bidi-theme-font:minor-bidi;}

Nanostructured Doped Silica Films Application as Sensitive Layers for Chemical Sensors

2013 ◽  
Vol 684 ◽  
pp. 7-11
Author(s):  
Sergey Krutovertsev ◽  
Alla Tarasova ◽  
Olga Ivanova ◽  
Larisa Krutovertseva
Keyword(s):  
Initial Conditions ◽  
Sol Gel ◽  
Silica Films ◽  
Adsorption Activity ◽  
Developed Surface ◽  
Sol Gel Process ◽  
Sensitive Characteristics ◽  
The Right ◽  
Kinetics Of ◽  
Matrix Factors

The sensor behavior of nanostructured doped silica films produced by sol-gel way were examined. Hygroscopic substances and polyoxometalates were used as additives to make more significant sensitive characteristics of initial matrix. Factors that have effect on sol preparation and films forming were investigated. Adsorption activity of the sensitive films was studied and it was shown that the films had a highly developed surface with nano-size pores. Change of initial conditions of sol-gel process gives opportunity to influence on kinetics of gel formation and consequently, on structure and properties of final materials. The study showed that the conditions of the environment affected the sensors characteristics markedly, which can be improved by choosing of the right procedure of forming and treatment. Influence of type and additive substances quantity into doped films was discussed in the paper

Preparation of Magnesium-Based Cobalt-Ferrites (Co1−xMgxFe2O4) Nanoparticles by Sol–Gel Auto Combustion Method

2017 ◽  
Vol 17 (01n02) ◽  
pp. 1760012
Author(s):  
S. Gowreesan ◽  
A. Ruban Kumar
Keyword(s):  
Particle Size ◽  
Structural Parameters ◽  
Sol Gel ◽  
Average Particle Size ◽  
Combustion Method ◽  
Dielectric Behavior ◽  
Powder Xrd ◽  
Average Particle ◽  
Cobalt Ferrites ◽  
Auto Combustion

The scope of the present work is in enhancing the particle size, and dielectric properties of Mg-substituted Cobalt ferrites nanoparticles prepared by sol–gel auto combustion method. The different ratios of Mg-substituted Co Ferrites (Co[Formula: see text]MgxFe2O4([Formula: see text], 0.05, 0.10, 0.15, 0.20 and 0.30)) are calcinated at 850[Formula: see text]C. The synthesized nanoparticles were characterized by powder XRD, FTIR, FE-SEM, EDX techniques and dielectric behavior. The structural parameters were confirmed from powder XRD and the average particle size is obtained from 39 to 67 nm due to the substitution of Mg[Formula: see text] which was calculated by Debye Scherrer’s formula. FE-SEM showed the surface morphology of the different ratio of the sample. The dielectric loss has measured the frequency range of 50[Formula: see text]Hz–5[Formula: see text]MHz. From electrical modulus, conductivity relaxation and thermal activation of charge carriers has been discussed.

Effect of Annealing Temperature on Phase Transition of Nanoalumina Synthesized by Auto-Combustion Route

2016 ◽  
Vol 41 ◽  
pp. 74-86 ◽  
Author(s):  
Muhammad Adil ◽  
Hasnah Mohd Zaid ◽  
Kean Chuan Lee ◽  
Noor Rasyada Ahmad Latiff
Keyword(s):  
Phase Transition ◽  
Particle Size ◽  
Sol Gel ◽  
Thermo Gravimetric Analysis ◽  
Amorphous State ◽  
Specific Area ◽  
Combustion Method ◽  
Gravimetric Analysis ◽  
Crystalline Phases ◽  
Auto Combustion

Nanocrystalline Al2O3 powder has been successfully synthesized by a simple and fast sol-gel auto-combustion method. The transformation of crystalline phases of as-synthesized nano powders was investigated through X-ray diffraction in terms of their crystallinity and crystallite size. Subsequently, a detailed transmission electron microscopy (TEM) investigation, including specific area electron diffraction (SAED) analysis revealed the crystallographic alterations and morphological information even at lattice scale which co-include the XRD analysis. The results obtained allow to explain the evolution of an amorphous state into different crystalline phases with increased calcining temperature; and their relation to particle size. The particle size is found to be closely related to phase transition of Al2O3 from γ → δ → θ → κ →α. The existence of distinctive bonds and band energy were studied by employing Fourier-transform infrared spectroscopy (FTIR) and UV-visible spectroscopy, respectively. On the other hand, thermo gravimetric analysis (TGA) had also been performed to confirm the phase purity of nano powder.

scholarly journals The use of Liquid Smoke as A Substitute for Nitric Acid for Extraction of Amorphous silica from Rice husk through Sol-Gel Route

2016 ◽  
Vol 32 (4) ◽  
pp. 2079-2085 ◽  
Author(s):  
Wasinton Simanjuntak ◽  
Simon Sembiring ◽  
Kamisah Kamisah ◽  
D. Pandiangan ◽  
Faradilla Syani ◽  
...  
Keyword(s):  
Nitric Acid ◽  
Rice Husk ◽  
Amorphous Silica ◽  
Sol Gel ◽  
Liquid Smoke

Fabrication and Microstructure of ZnO-TiO2 Composite Membranes by a Reverse Micelle and Sol-Gel Processing

2006 ◽  
Vol 510-511 ◽  
pp. 786-789 ◽  
Author(s):  
Dong Sik Bae ◽  
Byung Ik Kim ◽  
Kyong Sop Han
Keyword(s):  
Particle Size ◽  
Reverse Micelle ◽  
Porous Alumina ◽  
Sol Gel ◽  
Average Particle Size ◽  
Composite Membranes ◽  
Dip Coating ◽  
Narrow Particle Size Distribution ◽  
Average Particle ◽  
Alumina Support

ZnO-TiO2 nanoparticles were synthesized by a reverse micelle and sol-gel process. The average particle size of the colloid was below 30 nm and well dispersed in the solution. ZnOTiO2 composite membranes were fabricated by using the dip-coating method on a porous alumina support. ZnO-TiO2 composite membranes showed a crack-free microstructure and narrow particle size distribution even after the heat treatment up to 600°C. The average particle size of the membrane was 30-40nm, and the pore size of ZnO-TiO2 composite membrane was below 10 nm.

Rapid Synthesis and Characterization of Maghemite Nanoparticles

2008 ◽  
Vol 8 (2) ◽  
pp. 861-866 ◽  
Author(s):  
Bilsen Tural ◽  
Macit Özenbaş ◽  
Selçuk Atalay ◽  
Mürvet Volkan
Keyword(s):  
Particle Size ◽  
Elevated Temperatures ◽  
Sol Gel ◽  
Volume Ratio ◽  
Silica Matrix ◽  
Superparamagnetic Nanoparticles ◽  
Maghemite Nanoparticles ◽  
Gelation Temperature ◽  
Iron Oxide Particles ◽  
Evaporation Surface

Fe2O3–SiO2 nanocomposites were prepared by a sol–gel method using various evaporation surface to volume (S/V) ratios ranging from 0.03 to 0.2. The Fe2O3–SiO2 sols were gelated at various temperatures ranging from 50 °C to 70 °C, and subsequently they were calcined in air at 400 °C for 4 hours. The structure and the magnetic properties of the prepared Fe2O3–SiO2 nanocomposites were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), differential thermal analysis (DTA), and vibrating sample magnetometer (VSM) measurements. The gelation temperature of the Fe2O3–SiO2 sols influenced strongly the particle size and crystallinity of the maghemite nanoparticles. It was observed that the particle size of maghemite nanoparticles increased with the increasing of the gelation temperature of the sols, which may be due to the agglomeration of the maghemite particles at elevated temperatures inside the microporosity of the silica matrix during the gelation process, and the subsequent calcination of these gels at 400 °C resulted in the formation of large size iron oxide particles. Magnetization studies at temperatures of 10, 195, and 300 K showed superparamagnetic behavior for all the nanocomposites prepared using the evaporation surface to volume ratio (S/V) of 0.1, 0.2, 0.09, and 0.08. The saturation magnetization, Ms, values measured at 10K were 5.5, 8.5, and 9.5 emu/g, for the samples gelated at 50, 60, and 70 °C, respectively. At the gelation temperature of 70 °C, γ-Fe2O3 crystalline superparamagnetic nanoparticles with the particle size of 9±2 nm were formed in 12 hours for the samples prepared at the S/V ratio of 0.2.

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