Sol–gel synthesis and thermal behavior of bioactive ferrous citrate–silica hybrid materials

Imbalance of the iron level in the body causes several diseases. In particular, the low level of iron, during pregnancy, is responsible for the iron deficiency anemia, and even of neurodegenerative diseases. Although the treatment of iron deficiency anemia with oral iron supplements has been known, this problem still afflicts many people. The aim of this work was the development of a system able to release ferrous ions in a controlled manner. Controlled drug release for medical applications, indeed, appears to be a very interesting alternative to a systemic therapy because it is assurance of treatment continuity and drug stability and optimizes drug absorption. For this purpose, ferrous citrate (Fe(II)C) was synthesized by a redox reaction between iron powder and citric acid. Fourier transform infrared spectroscopy (FTIR), 1,10-phenanthroline and sodium thiocyanate colorimetric assays confirmed that only Fe(II)C was obtained by redox reaction. Afterward, obtained Fe(II)C was embedded within a SiO2 matrix in different mass percentage, by means of a sol–gel route. FTIR spectroscopy and simultaneous thermogravimetry/first-order derivative of thermogravimetry were used to confirm the Fe(II)C presence in the silica matrix and to investigate the thermal behavior of the sol–gel materials, respectively. The bioactivity test carried out by soaking the synthesized drug delivery systems in a simulated body fluid showed that the biological properties of the silica matrix are not modified by the presence of Fe(II)C

Sol-Gel synthesis, spectroscopic and thermal behavior study of SiO2/PEG composites containing different amount of chlorogenic acid

In this work, new phenol-based materials have been synthesized by the sol-gel method, in which different amounts of the phenolic antioxidant chlorogenic acid (CGA) (from 5 wt % to 20 wt %) were embedded in two different silica matrices: pure silica and silica-based hybrids materials, containing 50 wt % of polyethylene glycol (PEG). The incorporation of CGA in different sol-gel matrices might protect them from degradation, which could cause the loss of their properties. The two series of materials were chemically characterized by Fourier transform infrared (FTIR) spectroscopy. In addition, the thermal behavior of both series of materials containing CGA was studied by thermogravimetry under both air and inert N2flowing gas atmosphere. The bioactivity was evaluated by soaking the synthesized hybrids in a simulated body fluid, showing that the bioactivity of the silica matrix is not modified by the presence of PEG and CGA

Characterization of Hybrid Materials Prepared by Sol-Gel Method for Biomedical Implementations. A Critical Review

The interaction between tissues and biomaterials (BM) has the purpose of improving and replacing anatomical parts of the human body, avoiding the occurrence of adverse reactions in the host organism. Unfortunately, the early failure of implants cannot be currently avoided, since neither a good mixture of mechanical and chemical characteristics of materials nor their biocompatibility has been yet achieved. Bioactive glasses are recognized to be a fine class of bioactive substances for good repair and replacement. BM interact with living bones through the formation of a hydroxyapatite surface layer that is analogous to bones. Bioglasses’ composition noticeably affects their biological properties, as does the synthesis method, with the best one being the versatile sol-gel technique, which includes the change of scheme from a ‘sol’ fluid into a ‘gel’. This process is widely used to prepare many materials for biomedical implants (e.g., hip and knee prostheses, heart valves, and ceramic, glassy and hybrid materials to serve as carriers for drug release). Nanoparticles prepared by the sol-gel method are interesting systems for biomedical implementations, and particularly useful for cancer therapy. This review provides many examples concerning the synthesis and characterization of the above-mentioned materials either taken from literature and from recently prepared zirconia/polyethylene glycol (PEG) hybrids, and the corresponding results are extensively discussed

Thermal behavior and antibacterial studies of a carbonate Mg–Al-based layered double hydroxide (LDH) for in vivo uses

The goal of this work is to study the thermal behavior and the antibacterial properties of a MgAl-CO3 layered double hydroxide (LDH), which demonstrated high efficiency in removing chromium (VI) from contaminated industrial wastewater. The compound has been synthesized via co-precipitation route (direct method) followed by hydrothermal treatment, obtaining nanoscopic crystallites with a partially disordered (turbostratic) structure. After its synthesis, the compound was characterized by means of X-ray powder diffraction, field emission scanning electron microscope, inductively coupled plasma atomic emission spectroscopy and analysis and Fourier transform infrared spectroscopy. On the other hand, with the view to check the drug delivery and surgical tools usage of MgAl-CO3, antibacterial tests, performed according to the Kirby–Bauer method, revealed the inability the growth of the pathogenic bacterial strains. Thermogravimetry and differential thermal analysis revealed that evolution of water from the material occurs in two stages upon heating and a noticeable interaction takes place between water (in the vapor phase) and MgAl-CO3. Kinetic analysis of both steps provides almost constant values of activation energy, with the following average values in the range 0.1 < a < 0.9: E1 = (66 ± 9) kJ mol‒1; E2 = (106 ± 7) kJ mol‒1. Finally, prediction of reasonable reaction times extrapolated at 25 and 37 °C has been made from kinetic parameters of the first step, while almost unrealistic reaction time values were determined using the same procedure with kinetic parameters related to the second step

Thermal and spectroscopic (TG/DSC-FTIR) characterization of mixed plastics for materials and energy recovery under pyrolytic conditions

Seven waste thermoplastic polymers (polypropylene, polyethylene film, polyethylene terephthalate, polystyrene, acrylonitrile–butadiene–styrene, high-impact polystyrene and polybutadiene terephthalate, denoted as PP, PE (film), PET, PS, ABS, HIPS and PBT, respectively) and four synthetic mixtures thereof with different compositions representing commingled postconsumer plastic waste and waste of electrical and electronic equipment were studied by means of simultaneous thermogravimetry/differential scanning calorimetry coupled with Fourier transform infrared spectroscopy (TG/DSC–FTIR) under pyrolytic conditions (inert atmosphere). By summing all the heat change contributions due to physical and/or chemical processes occurring (i.e., melting, decomposition), an overall energy, defined as the degradation heat, was determined for both single component and their mixtures. It was found to be about 4–5 % of the exploitable energy of the input material. Vapors evolved during the pyrolysis of single-component polymers and their mixtures, analyzed using the FTIR apparatus, allowed identifying the main reaction products as monomers or fragments of the polymeric chain. Results from TG/DSC runs and FTIR analysis show that there is no interaction among the plastic components of the mixtures during the occurrence of pyrolysis

Thermal behavior study of pristine and modified halloysite nanotubes: A modern kinetic study

Pristine halloysite nanotubes (HNTs) were studied by thermogravimetry (TG) up to 800 C. Etching of alumina from inside the tube (causing a significant increase in tube lumen) was realized by treating the material with an acidic H2SO4 solution at 50 C. Both materials were characterized by TG-FTIR techniques and their thermal behaviors were compared with that of kaolinite. The coupling of TG with FTIR enables to detect the gases evolved during the TG experiments, thus confirming that only pristine HNTs undergo dehydration with the loss of interlayer water molecules at around 245 C, while dehydroxylation occurs in all these materials in close temperature ranges around 500 C. TG runs at five different heating rates (2, 5, 10, 15 and 20 C min-1), was carried out in the same experimental conditions used for the thermal analysis study with the aim to investigate dehydration and dehydroxylation kinetics using some isoconversional methods recommended by the ICTAC kinetic committee, and thermogravimetric data under a modulated rising temperature program. Finally, the results of the kinetic analysis were discussed and explained in terms of the strengths of the hydrogen bonds broken during these processes

Evaporation/decomposition behavior of 1-Butyl-3-Methylimidazolium Chloride (BMImCL) investigated through effusion and thermal analysis techniques

The evaporation/decomposition behavior of the ionic liquid 1-butyl-3-methylimidazolium chloride (BMImCl) was studied with various techniques, such as thermogravimetry (TG), Knudsen effusion mass loss (KEML), and Knudsen effusion mass spectrometry (KEMS), in order to investigate the competition between the simple evaporation of the liquid as gaseous ion pairs (NIP: neutral ion pair) and the thermal decomposition releasing volatile species. TG/DSC experiments were carried out from 293 to 823 K under both He and N2 flowing atmospheres on BMImCl as well as on BMImNTf2 (NTf2: bis(trifluoromethylsulfonyl)imide). Both ionic liquids were found undergoing a single step of mass loss in the temperature range investigated. However, while the BMImNTf2 mass loss was found to occur in different temperature ranges, depending on the inert gas used, the TG curves of BMImCl under helium and nitrogen flow were practically superimposable, thus suggesting the occurrence of thermal decomposition. Furthermore, KEML experiments on BMImCl (in the range between 398 and 481 K) indicated a clear dependence of the unit area mass loss rate on the effusion hole diameter, an effect not observed for the ILs with NTf2 anion. Finally, KEMS measurements in the 416–474 K range allowed us to identify the most abundant species in the vapor phase, which resulted in methyl chloride, butylimidazole, butyl chloride, and methylimidazole, which most probably formed from the decomposition of the liquid

Synthesis and characterization of a Mg–Ni-RE alloy for hydrogen storage

The synthesis and characterization of a Mg–Ni alloy having La and Ce as catalysts, have been performed. The alloy behavior was studied at given fixed temperature and pressure during hydrogen absorption/desorption tests. The La and Ce addition was carried out starting from a commercial alloy, named “Firesteel”. The alloy synthesized has the following formula Mg68Ni26M5X, where X represents Si and Fe impurities and M stands for the mixture of rare earths metals. The alloy has been prepared by a melting process in an induction furnace equipped with a centrifugal casting system and then grinded, by both hydraulic press and ball milling. The alloy has been characterized by SEM, BET, XRD, DSC-TGA analysis and by a mass flow measurement apparatus. The experiments on alloy sample showed that, after activation, hydrogenation occurs at 300 °C in three stages at three different pressures: 3, 4 and 7 atm, involving respectively 0.15 wt%, 0.4 wt% and 2.2 wt% of hydrogen absorbed. Reversible hydride dehydrogenation, inside the mass flow measurement apparatus, requires a working temperature of 350 °C to obtain, with remarkable reaction rate, about 2.7%, hydrogen desorption