Effect of acidity on the properties of silica-aluminas synthesized by sol-gel method

2020 ◽  
Vol 63 (7) ◽  
pp. 126-132
Author(s):  
Lyubov V. Furda ◽  
◽  
Evgenia A. Tarasenko ◽  
Sofya N. Dudina ◽  
Olga E. Lebedeva ◽  
...  
Keyword(s):  
Surface Area ◽  
Sol Gel ◽  
Molar Ratio ◽  
Active Centers ◽  
Indicator Method ◽  
Synthesis Conditions ◽  
Alkaline Conditions ◽  
Acidic Conditions ◽  
Amphoteric Properties ◽  
Hydrolysis Of

In the present work amorphous silica-aluminas were synthesized by the coprecipitation method during the hydrolysis of an alcohol solution of tetraethoxysilane (with a tetraethoxysilane: alcohol mass ratio of 1: 1) and 6% aqueous solution of aluminum nitrate at pH values of 1, 3, and 10. The Si/Al molar ratio for all synthesized samples were 4.72 (± 0.29). The amorphous character of the investigated materials was confirmed by X-ray phase analysis. According to the results of scanning electron microscopy, it was found that the resulting powders have particles with a size of 1-20 μm. It was shown that the conditions of synthesis affected the specific surface area and porosity of the materials under study. By the method of low-temperature adsorption-thermodesorption of nitrogen it was established that silica-aluminas obtained under acidic conditions were microporous materials. For the sample obtained under alkaline conditions (pH = 10), the contribution of macropores is very significant. A decrease in surface area is observed as the pH of the synthesis increases. The Hammett indicator method was used to identify and quantify surface centers of different acidity. All studied silica-aluminas are characterized by the presence of both Brønsted basic (pKax from 7 to 12.8) and acidic (pKax from 0 to 7) centers, and Lewis basic (pKax from -4.4 to 0) with a pronounced maximum at pKax = 1.02. It was found that the synthesis conditions had a significant effect on the concentration of active centers. The values of the Hammett function are practically the same for the 3 studied silica-aluminas and describe the studied samples as materials of medium acidity. The variety of Lewis and Brønsted centers on the surface indicates the amphoteric properties of the materials under study. This gives the samples the properties of polyfunctional sorbents and catalysts.

scholarly journals Sol-gel preparation and properties of amorphous iron-containing aluminosilicate

2020 ◽  
Vol 64 (11) ◽  
pp. 102-107
Author(s):  
Lyubov V. Furda ◽  
◽  
Evgeniya A. Tarasenko ◽  
Sofya N. Dudina ◽  
Olga E. Lebedeva ◽  
...  
Keyword(s):  
Specific Surface ◽  
Surface Area ◽  
Specific Surface Area ◽  
Active Sites ◽  
Sol Gel ◽  
Reference Sample ◽  
Acid Sites ◽  
Molar Ratio ◽  
Indicator Method ◽  
Gel Preparation

The objective of the present study includes a modification of synthetic aluminosilicate with iron cations and an estimation of the modificator influence at structure and properties of the aluminosilicate. The iron-containing aluminosilicate (Si/Al = 4.72) with an Al/Fe molar ratio of 5:1 was prepared by the sol-gel method at pH = 1-2. Amorphous aluminosilicate (Si/Al = 4.72), which was synthesized by analogous procedure, was applied as a reference sample. By scanning electron microscopy, it was found that the powders had particles of 1-20 micrometers in size. The results of low-temperature adsorption-thermal desorption of nitrogen showed that the modification with Fe3+ ions affected the specific surface area and porosity of the material under study. The iron-containing sample has a higher specific surface area and pore volume comparing to the initial aluminosilicate. The Hammett indicator method was used to evaluate the surface centers of the samples. It was found that the materials under study were characterized by the presence of active sites with pKax values in the range from - 4.4 to 12.8 with a pronounced maximum at pKax = 1.02. For an iron-containing sample, the concentration of acid sites significantly decreases at pKax = 1.02, while at pKax 0.80, 1.03, 2.10, 2.50, 4.10, 5.00, 8.00, and 12.80, an increase in the number of acid sites is observed. The values of the Hammett function are practically the same for the studied samples and characterizes them as materials of medium acidity. For iron-containing aluminosilicate, the larger number of active sites was noted, it amounted to 313.5 mmol/g.

Relation between Surface Area and Surface Potential Change during (co)Polyesters Degradation as Langmuir Monolayer

MRS Advances ◽  
2019 ◽  
Vol 5 (12-13) ◽  
pp. 667-677
Author(s):  
Natalia A. Tarazona ◽  
Rainhard Machatschek ◽  
Andreas Lendlein
Keyword(s):  
Surface Area ◽  
Surface Potential ◽  
Degradation Products ◽  
Degradation Mechanism ◽  
Langmuir Monolayers ◽  
Langmuir Monolayer ◽  
Potential Change ◽  
Alkaline Conditions ◽  
Hydrolysis Of ◽  
Random Scission

ABSTRACTPolyhydroxyalkanoates (PHAs) are degradable (co)polyesters synthesized by microorganisms with a variety of side-chains and co-monomer ratios. PHAs can be efficiently hydrolyzed under alkaline conditions and by PHA depolymerase enzymes, altering their physicochemical properties. Using 2D Langmuir monolayers as model system to study the degradation behavior of macromolecules, we aim to describe the the interdependency between the degradation of two PHAs and the surface potential, which influences material-proteins interaction and cell response. We hypothesize that the mechanism of hydrolysis of the labile ester bonds in (co)polyesters defines the evolution of the surface potential, owing to the rate of accumulation of charged insoluble degradation products. The alkaline hydrolysis and the enzymatically catalyzed hydrolysis of PHAs were previously defined as chain-end scission and random-scission mechanisms, respectively. In this study, these two distinct scenarios are used to validate our model. The surface potential change during the chain-end scission of poly(3-R-hydroxybutyrate) (PHB) under alkaline conditions was compared to that of the enzymatically catalyzed hydrolysis (random-scission) of poly[(3-R-hydroxyoctanoate)-co-(3-R-hydroxyhexanoate)] (PHOHHx), using the Langmuir monolayer technique. In the random-scission mechanism the dissolution of degradation products, measured as a decrease in the area per molecule, was preceded by a substantial change of the surface potential, provoked by the negative charge of the broken ester bonds accumulated in the air-water interface. In contrast, when chains degraded via the chain-ends, the surface potential changed in line with the dissolution of the material, presenting a kinetic dependent on the surface area of the monolayers. These results provide a basis for understanding PHAs degradation mechanism. Future research on (co)polymers with different main-chain lengths might extend the elucidation of the surface potential development of (co)polyesters as Langmuir monolayer.

Effect of the Sol-Gel Synthesis Parameters on the Incorporation of an Anti-inflammatory Drug in a Ceramic Material

2007 ◽  
Vol 1007 ◽  
Author(s):  
Aracely Hernandez ◽  
Patricia Esquivel-Ferriño ◽  
Idalia Gomez ◽  
Lucia Cantu
Keyword(s):  
Ceramic Material ◽  
Sol Gel ◽  
Nitrogen Adsorption ◽  
Molar Ratio ◽  
Inflammatory Drug ◽  
Synthesis Conditions ◽  
Synthesis Parameters ◽  
Anti Inflammatory ◽  
Drug Incorporation ◽  
Sol Gel Synthesis

ABSTRACTIn the present work, sol-gel method was used to incorporate in a ceramic material a non steroidal anti-inflammatory drug (piroxicam) as model drug. The incorporation of the drug in the SiO2 network was carried out at different sol-gel synthesis parameters, such as pH (3 and 5) and the alkoxide/water ratio (1:6 and 1:8). The biomaterial obtained was analyzed by thermal analysis TGA-DTA, infrared spectroscopy (FTIR), Scanning Electronic Microscopy (SEM) and X-ray diffraction (XRD); specific surface area and porosity were analyzed from nitrogen adsorption isotherm. Better drug incorporation into the material was achieved at the synthesis conditions of pH 5 and 1:6 alkoxide/water molar ratio.

Preparation and Characterization of Ultralow Density Silica Aerogels by Acetonitrile Supercritical Drying

2012 ◽  
Vol 519 ◽  
pp. 83-86 ◽  
Author(s):  
Guang Wu Liu ◽  
Xing Yuan Ni ◽  
Bin Zhou ◽  
Qiu Jie Yu
Keyword(s):  
Specific Surface ◽  
Surface Area ◽  
Specific Surface Area ◽  
Silica Aerogel ◽  
Sol Gel ◽  
Supercritical Drying ◽  
Silica Aerogels ◽  
High Specific Surface Area ◽  
Molar Ratio ◽  
Sol Gel Process

This paper deals with the synthesis of ultralow density silica aerogels using tetramethyl orthosilicate (TMOS) as the precursor via sol-gel process followed by supercritical drying using acetonitrile solvent extraction. Ultralow density silica aerogels with 6 mg/cc of density was made for the molar ratio by this method. The microstructure and morphology of the ultralow density silica aerogels was characterized by the specific surface area, SBET, SEM, and the pore size distribution techniques. The results show that the ultralow density silica aerogel has the high specific surface area of 812m2/g. Thermal conductivities at desired temperatures were analyzed by the transient plane heat source method. Thermal conductivity coefficients of silica aerogel monoliths changed from 0.024 to 0.043W/ (m K) as temperature increased to 400°C, revealed an excellent heat insulation effect during thermal process.

scholarly journals Synthesis of Silica Nanostructures and Optimization of their Size and Morphology by Use of Changing in Synthesis Conditions

2012 ◽  
Vol 9 (2) ◽  
pp. 659-668 ◽  
Author(s):  
A. Elsagh
Keyword(s):  
Drug Delivery Systems ◽  
Sol Gel ◽  
Molar Ratio ◽  
Synthesis Conditions ◽  
Acid Type ◽  
Silica Nanostructures ◽  
Size And Morphology ◽  
Sol Gel Synthesis ◽  
Optimized Conditions ◽  
Cracking Products

The aim of the present research was optimization of practical conditions of the sol-gel synthesis. In so doing, silica particles were synthesized using sol-gel method and their size and morphology were investigated by use of SEM and TEM images. The effect of changing molar ratio of reactive including acids and silica pre-matter on the particles' morphology and size was studied. Also, acid type and silica pre-matter used in reaction was examined and the result product of the reaction were investigated in the presence of several acids and two types of silica pre-matter. The reaction time was studied as a very important factor in products' digestion phase which plays a significant role in determining particles’ size and rate of cracking products. Finally, in optimized conditions 50-80 nm diameter nanostructures were synthesized. These products can be used as drug delivery systems.

Synthesis and Structural Characterization of SiO2-Al2O3 Xerogels

2007 ◽  
Vol 336-338 ◽  
pp. 2286-2289
Author(s):  
Fei He ◽  
Xiao Dong He ◽  
Yao Li
Keyword(s):  
Structural Change ◽  
Specific Surface ◽  
Surface Area ◽  
Specific Surface Area ◽  
Sol Gel ◽  
Nitrogen Adsorption ◽  
Mesoporous Structure ◽  
Supercritical Drying ◽  
High Specific Surface Area ◽  
Molar Ratio

Low-density xSiO2-(1-x)Al2O3 xerogels with x=0.9, 0.8, 0.7, 0.6 (mole fractions) were prepared by sol-gel and non-supercritical drying. Silica alkogels, which were the framework of binary composite materials, formed from tetraethyl orthosilicate (TEOS) by hydrolytic condensation with a molar ratio of TEOS: H2O: alcohol: hydrochloric acid: ammonia =1: 4: 10: 7.5×10-4: 0.0375. Aluminum hydroxide derived from Al(NO3)3·9H2O and NH4OH acting in the alcohol solution under the condition of catalyst. After filtrating and washing, the precipitation was mixed into silica sols to form SiO2-Al2O3 mixed oxide gels with different silicon and aluminum molar ratio. The structural change and crystallization of the binary xerogels were investigated after heat treatment at 600 for 2 h by the means of X-ray diffraction. Nitrogen adsorption experiment was performed to estimate specific surface area, porous volume and pore size distribution. The structural change of xerogels was observed by FT-IR spectroscopy. The resulting mixed xerogels possess of mesoporous structure which is characteristic of cylindrical pores, high specific surface area of 596-863 m2/g and a relatively narrow pore distribution of 2.8-30 nm. Al2O3 is introduced into the SiO2 phase and some of Al-O-Si bonds form.

A Direct Route to Active Silica Nanoparticles

2007 ◽  
Vol 121-123 ◽  
pp. 65-68
Author(s):  
X.Q. Chen ◽  
Y.Y. Liu ◽  
K.H. Qi ◽  
X. Zhou ◽  
J.H. Xin
Keyword(s):  
Aqueous Solution ◽  
Silica Nanoparticles ◽  
Sol Gel ◽  
Silica Particles ◽  
Second Step ◽  
Gel Method ◽  
Direct Route ◽  
Monodisperse Silica ◽  
Acidic Conditions ◽  
Hydrolysis Of

Monodisperse silica particles containing available active C=C bonds were directly prepared by a simple two-step sol-gel method. In the first step the hydrolysis of vinyltrimethoxysilane (VTMS) was performed under acidic conditions in an aqueous solution. In the second step the condensation of the siloxane precursors progressed under basic conditions, resulting in production of silica nanoparticles containing available active C=C bonds. The products were characterized using SEM and FTIR.

scholarly journals PVP-Stabilized Palladium Nanoparticles in Silica as Effective Catalysts for Hydrogenation Reactions

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Caroline Pires Ruas ◽  
Daiane Kessler Fischer ◽  
Marcos Alexandre Gelesky
Keyword(s):  
Catalytic Activity ◽  
Palladium Nanoparticles ◽  
Sol Gel ◽  
Molar Ratio ◽  
Sol Gel Process ◽  
Hydrogenation Reactions ◽  
Acidic Conditions

Palladium nanoparticles stabilized by poly (N-vinyl-2-pyrrolidone) (PVP) can be synthesized by corresponding Pd(acac)2(acac = acetylacetonate) as precursor in methanol at 80°C for 2 h followed by reduction with NaBH4and immobilized onto SiO2prepared by sol-gel process under acidic conditions (HF or HCl). The PVP/Pd molar ratio is set to 6. The effect of the sol-gel catalyst on the silica morphology and texture and on Pd(0) content was investigated. The catalysts prepared (ca.2% Pd(0)/SiO2/HF andca.0,3% Pd(0)/SiO2/HCl) were characterized by TEM, FAAS, and SEM-EDS. Palladium nanoparticles supported in silica with a size 6.6 ± 1.4 nm were obtained. The catalytic activity was tested in hydrogenation of alkenes.

Preparation of a Silicon Oximide Gel via a Non-Aqueous Sol-Gel Route

2002 ◽  
Vol 726 ◽  
Author(s):  
Fei Cheng ◽  
John S. Bradley
Keyword(s):  
Amorphous Silicon ◽  
Surface Area ◽  
Sol Gel ◽  
Total Surface Area ◽  
Mas Nmr ◽  
Bet Surface Area ◽  
Molar Ratio ◽  
Microporous Structure ◽  
Silicon Oxycarbonitride ◽  
Cp Mas Nmr

AbstractA silicon oximide gel was prepared by a reaction in N,N-dimethylformamide between tris(dimethylamino)silylamine (Me2N)3SiNH2 (TDSA) and formamide in a 1:2 molar ratio at 50C. The 29Si, 13C CP-MAS NMR and IR analyses indicated that the gel mainly comprised oximino silicon networks [SiOC(H)=NSi]x. The gel exhibited a microporous structure and had a total surface area of 339 m2/g. A microporous structure with a BET surface area of 195 m2/g was also obtained after pyrolysis of the gel at 1000°C for 2 h. Pyrolysis of the gel under N2 up to 1485°C gave an amorphous silicon oxycarbonitride glass.

Preparation of Multicomponent Ceramic Powders by Sol-Gel Processing

1990 ◽  
Vol 180 ◽  
Author(s):  
J.R. Bartlett ◽  
J.L. Woolfrey
Keyword(s):  
Electron Microscopy ◽  
Sol Gel ◽  
Processing Conditions ◽  
X Ray Diffraction ◽  
Ceramic Powders ◽  
X Ray ◽  
Acidic Conditions ◽  
Powder Properties ◽  
Gel Processing ◽  
Hydrolysis Of

ABSTRACTSol-gel methods have been applied to the production of the multicomponent ceramic, Synroc B. These techniques involved the hydrolysis of a mixture of Ti and Zr, alkoxides peptising to form a sol and subsequent sorption of Al3+, Ba2+ and Ca2+ cations under acidic conditions. Powder properties were examined by a variety of techniques, including electron microscopy, x-ray diffraction, N2 sorption, and differential thermal analysis. The effects of processing conditions on the physical properties of the powders are discussed.

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