Search results for "Thermogravimetric analysi"
showing 10 items of 213 documents
Interaction of Ni/SiO2 with thiophene.
2009
Abstract The interaction between Ni/SiO 2 (18 wt%) and thiophene was studied by thermal gravimetric analysis (TGA) and in a fixed-bed reactor. The samples were prepared by incipient wetness impregnation and reaction was realized in hydrogen flow at 280–360 °C in the presence of 10–40 mbar of thiophene. It is found that sulfidation of Ni is not complete in TGA experiments and the maximum achievable transformation degree depends not only on the temperature and thiophene pressure, but also on the sample weight and the gas flow rate. The maximum transformation degree is shown to vary reversibly when conditions are changed. Analysis of the reaction products during sulfidation in a fixed-bed reac…
Oxadiazolyl-pyridines and perfluoroalkyl-carboxylic acids as building blocks for protic ionic liquids: crossing the thin line between ionic and hydro…
2012
A series of 18 samples has been prepared in order to obtain fluorinated materials as Protic Ionic Liquids (PILs). These were synthesized by appropriately mixing 1,2,4-oxadiazoles derivatised with two pyridines, or one pyridine and a fluorinated chain, and perfluoroalkyl-carboxylic acids, either mono- or dicarboxylic, leading to symmetric and non-symmetric materials. Many of them showed low melting points. However, the possibility of classifying the synthesized materials as PILs is discussed in terms of effective ionicity of the systems by the combination of Density Functional Theory (DFT) calculation and IR spectroscopy. The important outcome of our investigation is that the complete proton…
A Straightforward Approach to Multifunctional Graphene
2019
Graphene has been covalently functionalized through a one-pot reductive pathway using graphite intercalation compounds (GICs), in particular KC8 , with three different orthogonally protected derivatives of 4-aminobenzylamine. This novel multifunctional platform exhibits excellent bulk functionalization homogeneity (Hbulk ) and degree of addition while preserving the chemical functionalities of the organic addends through different protecting groups, namely: tert-butyloxycarbonyl (Boc), benzyloxycarbonyl (Cbz) and phthalimide (Pht). We have employed (temperature-dependent) statistical Raman spectroscopy (SRS), X-ray photoelectron spectroscopy (XPS), magic angle spinning solid state 13 C NMR …
Carbon Nano-onions: Potassium Intercalation and Reductive Covalent Functionalization
2021
Herein we report the synthesis of covalently functionalized carbon nano-onions (CNOs) via a reductive approach using unprecedented alkali-metal CNO intercalation compounds. For the first time, an in situ Raman study of the controlled intercalation process with potassium has been carried out revealing a Fano resonance in highly doped CNOs. The intercalation was further confirmed by electron energy loss spectroscopy and X-ray diffraction. Moreover, the experimental results have been rationalized with DFT calculations. Covalently functionalized CNO derivatives were synthesized by using phenyl iodide and n-hexyl iodide as electrophiles in model nucleophilic substitution reactions. The functiona…
Adsorption isotherms and thermal behavior of hybrids based on quercetin and inorganic fillers
2019
We investigated the adsorption process of quercetin onto several inorganic fillers, such as kaolinite, calcium carbonate and alumina. Firstly, we performed equilibrium adsorption studies in order to determine the quercetin/filler adsorption isotherms, which were successfully fitted through the Langmuir model. Based on the adsorption data analysis, we estimated the maximum adsorption capacity of each filler as well as the Langmuir constant, which is related to the affinity between quercetin and the surfaces of the inorganic particles. Then, we prepared hybrids formed by fillers saturated with quercetin. The obtained composites were characterized by thermogravimetric analysis with the aim of …
Pineapple peel biochar and lateritic soil as adsorbents for recovery of ammonium nitrogen from human urine.
2021
Abstract Human urine is a rich source of nitrogen which can be captured to supplement the existing sources of nitrogen fertilizers thus contributing to enhanced crop production. However, urine is the major contributor of macronutrients in municipal wastewater flows resulting into eutrophication of the receiving water bodies. Herein, pineapple peel biochar (PPB), and lateritic soil (LS) adsorbents were prepared for the safe removal of ammonium nitrogen (NH4+-N) from human urine solutions. Physicochemical properties of PPB, and LS were characterized by scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS), X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy…
MCM-41 silica effect on gel polymer electrolytes based on thermoplastic polyurethane
2012
Abstract Polymer electrolytes were prepared from thermoplastic polyurethane with addition of mixture of N-ethyl(methylether)-N-methylpyrrolidinium trifluoromethanesulfonimide (PYRA12O1TFSI) ionic liquid, lithium bis(trifluoromethanesulfoneimide) salt and propylene carbonate. MCM-41 mesoporous silica was added in proportions ranging from 5 to 20 wt.% with respect to TPU. The electrolytes were characterized by thermogravimetric analysis, differential scanning calorimetry, linear voltammetry and impedance spectroscopy. The MCM-41 addition to the system was found to improve the electrochemical stability of the membranes and to reduce the gel electrolyte/metallic Li interfacial resistance. The f…
Microwave assisted synthesis and solid-state characterization of lithocholyl amides of isomeric aminopyridines
2011
Microwave (MW) assisted synthesis and solid state structural characterizations of novel lithocholyl amides of 2-, 3-, and 4-aminopyridine are reported. It is shown that the MW technique is a proper method in the preparation of N-lithocholyl amides of isomeric aminopyridines. It offers many advantages compared to conventional heating. The molecular and crystal structures as well as the polymorphic and hydrated forms of prepared conjugates with their thermodynamic stabilities have been characterized by means of high resolution liquid- and solid-state NMR spectroscopy, single crystal and powder X-ray diffraction, and thermogravimetric analysis. Owing to the many biological functions of bile ac…
Surface modification of luminescent lanthanide phosphate nanorods with cationic "Quat-primer" polymers.
2011
"Quat-primer" polymers bearing cationic groups were investigated as a surface modifier for Tb-doped cerium phosphate green-emitting fluorescent nanorods (NRs). The NRs were synthesized by a microwave process without using any complex agents or ligands and were characterized with different analytical tools such as X-ray diffraction, transmission electron microscopy, and fluorescence spectroscopy. Poly(ethyleneimine) partially quarternized with glycidyltrimethylammonium chloride was synthesized separately and characterized in detail. (1)H and (13)C NMR spectroscopic studies revealed that the quaternary ammonium group was covalently attached to the polymer. UV-vis spectroscopy was used to exam…
Comparison of Permeation Measurements and Hybrid Density Functional Calculations on Oxygen Vacancy Transport in Complex Perovskite Oxides
2014
The oxygen vacancy (VO••) formation enthalpy (ΔHF) was determined from the effective activation energies obtained in the permeation measurements on a series of solid solutions La0.98–xSrxCo0.2Fe0.8O3−δ (x = 0.125–0.8) and compared with the results of ab initio calculations at finite temperatures based on the hybrid (PBE0) and GGA+U calculations, as well as previous thermogravimetric experiments. The Mulliken atomic charges, magnetic moments, and the Fe-VO•• and Sr-VO•• distances are analyzed. The strong dependence of formation enthalpy of VO•• on the Fe oxidation state due to variation in Sr and VO•• concentrations is discussed.