Study of the influence of various solvents on the properties of hydrophobic silica xerogels

Silica aerogels are low-density inorganic aerogels with a three-dimensional nanoporous structure. Due to the inherent properties of nanoporous materials, the possibility of using silica airgel is of great interest in various fields. To simplify the process and reduce costs, the use of atmospheric pressure drying (APD) is promising, the resulting materials are called xerogels. Silica xerogels based on methyltrimethoxysilane were synthesized using various alcohol solvents. The optimal combination of properties is possessed by a sample obtained using methanol as a solvent. The wetting angle of all xerogels was 158°, which characterizes the resulting material as superhydrophobic.

Facile synthesis of high purity silica xerogel from rice straw

This research aims to synthesize a silica xerogel from rice straw that is a residue biomass generating from agriculture. Purity and morphological structure of synthesized silica xerogel are also studied. The first step of the synthesis is the preparation of sodium silicate from rice straw ash that is then used as silica source. To prepare a silica source, pretreated rice straw was burnt at 700 °C for 2 h to obtain a rice straw ash. After that resulted rice straw ash is washed and reacted with 1.0 M HCl and 2.0 M NaOH aqueous solution at 80 °C for 1 h, respectively. The reacted solution is then filtrated two times by a no.41 filter paper and ion exchange resin, respectively. The obtained sodium silicate is mixed with 1.0 M HCl under stirring for 6 h to produce the nano-silica. To increase the purity of nano-silica xerogels, as-synthesized silica was washed with deionized water for 3 times. Washed silica is dried in electric oven at 85 °C overnight and calcined at 500 °C for 5 h. Scanning electron microscopy/energy dispersive x-ray spectrometry (SEM/EDS) and % whiteness are employed to evaluate the morphology and purity of particles. Experimental results showed that nano-silica with purity up to 99.0 wt% was completely synthesized. Different morphological structure of silica synthesized under pH of 7, 8 and 9 were obtained.

Modification of Silica Xerogels with Polydopamine for Lipase B from Candida Antarctica Immobilization

Silica xerogels have been proposed as a potential support to immobilize enzymes. Improving xerogels’ interactions with such enzymes and their mechanical strengths is critical to their practical applications. Herein, based on the mussel-inspired chemistry, we demonstrated a simple and highly effective strategy for stabilizing enzymes embedded inside silica xerogels by a polydopamine (PDA) coating through in-situ polymerization. The modified silica xerogels were characterized by scanning and transmission electron microscopy, Fourier tranform infrared spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy and pore structure analyses. When the PDA-modified silica xerogels were used to immobilize enzymes of Candida antarctica lipase B (CALB), they exhibited a high loading ability of 45.6 mg/gsupport, which was higher than that of immobilized CALB in silica xerogels (28.5 mg/gsupport). The immobilized CALB of the PDA-modified silica xerogels retained 71.4% of their initial activities after 90 days of storage, whereas the free CALB retained only 30.2%. Moreover, compared with the immobilization of enzymes in silica xerogels, the mechanical properties, thermal stability and reusability of enzymes immobilized in PDA-modified silica xerogels were also improved significantly. These advantages indicate that the new hybrid material can be used as a low-cost and effective immobilized-enzyme support.

Silica Xerogel Doped with Iron(III) as Sensor Material for Salicylhydroxamic Acid Determination in Urine

Salicylhydroxamic acid (SHA) is used as antimicrobic medicine and its concentration has to be monitored in urine. For the first time, silica xerogels doped with iron(III) have been proposed as sensor materials for SHA determination in biological samples. Three xerogels with iron(III) content in the range of 0.04–1.74% wt have been synthesized. BET surface area of these xerogels has varied in the range of 696–529 m2/g and total pore volume has varied in the range of 0.92–0.23 cm3/g. Complex formation between immobilized iron(III) and salicylhydroxamic acid has been investigated with solid phase spectrophotometry and IR spectroscopy. Orange-brown iron(III)-SHA complex with 1:1 stoichiometry is formed at pH 1–4 with half-reaction time of 17 min. Silica xerogel doped with 0.33% wt iron(III)) has been used as sensor material for SHA solid phase spectrophotometric determination (LOD 1.4 mg/L (n = 3), analytical range 4–230 mg/L). Proposed sensor material has been applied for SHA determination in biological samples of synthetic and human urine. The proposed procedure is characterized by a good level of accuracy (recovery values 97–120%) and precision (RSD values 4–9%) and can be recommended for pharmacokinetic–pharmacodynamic studies of hydroxamic acid-based medications.

Butyl-Methyl-Pyridinium Tetrafluoroborate Confined in Mesoporous Silica Xerogels: Thermal Behaviour and Matrix-Template Interaction

Organic-inorganic silica composites have been prepared via acid catalyzed sol-gel route using tetramethoxysilan (TMOS) and methyl-trimethoxysilane (MTMS) as silica precursors and n-butyl-3-methylpyridinium tetrafluoroborate ([bmPy][BF4]) as co-solvent and pore template, by varying the content of the ionic liquid (IL). Morphology of the xerogels prepared using the ionic liquid templating agent were investigated using scanning electron microscopy and small angle neutron scattering (SANS). Thermal analysis has been used in order to evaluate the thermal and structural stability of the materials, in both nitrogen and synthetic air atmosphere. In nitrogen atmosphere, the IL decomposition took place in one step starting above 150 °C and completed in the 150–460 °C temperature interval. In synthetic air atmosphere, the IL decomposition produced two-step mass loss, mainly in the 170–430 °C temperature interval. The decomposition mechanism of the IL inside the silica matrix was studied by mass spectrometric evolved gas analysis (MSEGA). The measurements showed that the degradation of the IL’s longer side chain (butyl) starts at low temperature (above 150 °C) through a C-N bond cleavage, initiated by the nucleophilic attack of a fluorine ion.

Physicochemical Characterization and Drug Release Properties of Methyl-Substituted Silica Xerogels Made Using Sol–Gel Process

In this work, a multi-analytical approach involving nitrogen porosimetry, small angle neutron and X-ray scattering, Fourier transform infrared (FTIR) and nuclear magnetic resonance (NMR) spectroscopies, X-ray diffraction, thermal analysis and electron microscopy was applied to organically modified silica-based xerogels obtained through the sol–gel process. Starting from a tetraethoxysilane (TEOS) precursor, methyltriethoxysilane (MTES) was added to the reaction mixture at two different pH values (2.0 and 4.5) producing hybrid xerogels with different TEOS/MTES molar ratios. Significant differences in the structure were revealed in terms of the chemical composition of the silica network, hydrophilic/hydrophobic profile, particle dimension, pore shape/size and surface characteristics. The combined use of structural characterization methods allowed us to reveal a relation between the cavity dimensions, the synthesis pH value and the grade of methyl substitution. The effect of the structural properties on the controlled Captopril release efficiency has also been tested. This knowledge facilitates tailoring the pore network for specific usage in biological/medical applications. Knowledge on structural aspects, as reported in this work, represents a key starting point for the production of high-performance silica-based hybrid materials showing enhanced efficacy compared to bare silica prepared using only TEOS.

Physicochemical Properties of Mesoporous Organo-Silica Xerogels Fabricated through Organo Catalyst

The physicochemical properties of organo-silica xerogels derived from organo catalyst were pervasively investigated, including the effect of one-step catalyst (citric acid) and two-step catalyst (acid-base), and also to observe the effect of sol pH of organo-silica xerogel toward the structure and deconvolution characteristic. The organo-silica xerogels were characterized by FTIR, TGA and nitrogen sorption to obtain the physicochemical properties. The silica sol–gel method was applied to processed materials by employing TEOS (tetraethyl orthosilicate) as the main precursor. The final molar ratio of organo-silica was 1:38:x:y:5 (TEOS:ethanol: citric acid: NH3:H2O) where x is citric acid concentration (0.1–10 × 10−2 M) and y is ammonia concentration (0 to 3 × 10−3 M). FTIR spectra shows that the one-step catalyst xerogel using citric acid was handing over the higher Si-O-Si concentration as well as Si-C bonding than the dual catalyst xerogels with the presence of a base catalyst. The results exhibited that the highest relative area ratio of silanol/siloxane were 0.2972 and 0.1262 for organo catalyst loading at pH 6 and 6.5 of organo-silica sols, respectively. On the other hand, the organo-silica matrices in this work showed high surface area 546 m2 g−1 pH 6.5 (0.07 × 10−2 N citric acid) with pore size ~2.9 nm. It is concluded that the xerogels have mesoporous structures, which are effective for further application to separate NaCl in water desalination.

Hybrid Xerogels: Study of the Sol-Gel Process and Local Structure by Vibrational Spectroscopy

The properties of hybrid silica xerogels obtained by the sol-gel method are highly dependent on the precursor and the synthesis conditions. This study examines the influence of organic substituents of the precursor on the sol-gel process and determines the structure of the final materials in xerogels containing tetraethyl orthosilicate (TEOS) and alkyltriethoxysilane or chloroalkyltriethoxysilane at different molar percentages (RTEOS and ClRTEOS, R = methyl [M], ethyl [E], or propyl [P]). The intermolecular forces exerted by the organic moiety and the chlorine atom of the precursors were elucidated by comparing the sol-gel process between alkyl and chloroalkyl series. The microstructure of the resulting xerogels was explored in a structural theoretical study using Fourier transformed infrared spectroscopy and deconvolution methods, revealing the distribution of (SiO)4 and (SiO)6 rings in the silicon matrix of the hybrid xerogels. The results demonstrate that the alkyl chain and the chlorine atom of the precursor in these materials determines their inductive and steric effects on the sol-gel process and, therefore, their gelation times. Furthermore, the distribution of (SiO)4 and (SiO)6 rings was found to be consistent with the data from the X-Ray diffraction spectra, which confirm that the local periodicity associated with four-fold rings increases with higher percentage of precursor. Both the sol-gel process and the ordered domains formed determine the final structure of these hybrid materials and, therefore, their properties and potential applications.