Karolina Szwarc-Rzepka

Preparation of chitin-silica composites by in vitro silicification of two-dimensional Ianthella basta demosponge chitinous scaffolds under modified Stöber conditions.

Chitin is a biopolymer found in cell walls of various fungi and skeletal structures of numerous invertebrates. The occurrence of chitin within calcium- and silica-containing biominerals has inspired development of chitin-based hybrids and composites in vitro with specific physico-chemical and material properties. We show here for the first time that the two-dimensional α-chitin scaffolds isolated from the skeletons of marine demosponge Ianthella basta can be effectively silicified by the two-step method with the use of Stöber silica micro- and nanodispersions under Extreme Biomimetic conditions. The chitin-silica composites obtained at 120 °C were characterized by the presence of spherical SiO2 particles homogeneously distributed over the chitin fibers, which probably follows from the compatibility of Si-OH groups to the hydroxyl groups of chitin. The biocomposites obtained were characterized by various analytical techniques such as energy dispersive spectrometry, scanning electron microscopy, thermogravimetric/differential thermal analyses as well as X-ray photoelectron spectroscopy, Fourier transform infrared and Raman spectroscopy to determine possible interactions between silica and chitin molecule. The results presented proved that the character and course of the in vitro chitin silicification in Stöber dispersions depended considerably on the degree of hydrolysis of the SiO2 precursor.

Preparation and characterization of multifunctional chitin/lignin materials

Multifunctional chitin/lignin materials were synthesized. In order to combine mechanical milling of the biopolymers with simultaneous mixing, a centrifugal ball mill was utilized. The resulting materials, differing in terms of the proportions of precursors used, underwent detailed physicochemical and dispersive-morphological analysis. On the basis of FT-IR spectra and results of elemental analysis, the efficiency of the preparation of the materials was determined. The influence of the precursors on the thermal stability of the resulting systems was also evaluated. Zeta potential was determined as a function of pH to describe the electrokinetic stability of aqueous dispersions. This is important for evaluating the utility of the materials and indirectly confirms the effectiveness of the proposed method of synthesis of chitin/lignin products. Measurements were performed to determine basic colorimetric parameters, crucial in the production technology of multiple colored materials. It is expected that chitin/lignin materials will find a wide range of applications (biosorbents, polymer fillers, and electrochemical sensors), as they combine the unique properties of chitin with the specific structural features of lignin to provide a multifunctional material.

Epoxy Resin Composite Based on Functional Hybrid Fillers

A study was carried out involving the filling of epoxy resin (EP) with bentonites and silica modified with polyhedral oligomeric silsesquioxane (POSS). The method of homogenization and the type of filler affect the functional and canceling properties of the composites was determined. The filler content ranged from 1.5% to 4.5% by mass. The basic mechanical properties of the hybrid composites were found to improve, and, in particular, there was an increase in tensile strength by 44%, and in Charpy impact strength by 93%. The developed hybrid composites had characteristics typical of polymer nanocomposites modified by clays, with a fine plate morphology of brittle fractures observed by SEM, absence of a plate separation peak in Wide Angles X-ray Scattering (WAXS) curves, and an exfoliated structure observed by TEM.

Immobilization of multifunctional silsesquioxane cage on precipitated silica supports

Synthesis of octakis({3-glycidoxypropyl}dimethylsiloxy) octasilsesquioxane (G-POSS) was carried out based on a reaction involving the hydrosilylation of allyl glycidyl ether with octakis(dimethylsiloxy) octasilsesquioxane, using Karstedt’s catalyst and toluene. SiO2/POSS hybrid systems were obtained via a method of immobilization by evaporation of the solvent, using hydrated or spherical silica obtained by precipitation in an aqueous or emulsion environment. The surface of the SiO2 was modified using octakis({3-glycidoxypropyl}dimethylsiloxy) octasilsesquioxane (G-POSS). The effectiveness of the modification of the obtained hybrid materials was verified using Fourier transform infrared spectroscopy and nuclear magnetic resonance (29Si and 13C CP MAS NMR). The tests showed that the interactions between the silica support and the modifier are of the nature of chemical adsorption. In addition a mechanism was proposed for the interactions between silica and oligosilsesquioxane. To test the final effect, the hybrid systems were subjected to morphological evaluation (transmission electron microscopy). Parameters of porous structure of the products were also determined: the specific surface area, pore diameter and pore volume. Thermal stability was tested for the pure silsesquioxane cage, the initial silica supports and the resulting systems. Elemental analysis was also carried out to determine the effect of surface modification on the degree of coverage with a particular POSS compound.

Silica/lignosulfonate hybrid materials: Preparation and characterization

The research reported here concerns the synthesis, characterization and potential applications of silica/lignosulfonate hybrid materials. Three types of silica were used (Aerosil®200, Syloid®244 and hydrated silica), along with magnesium lignosulfonate. The effectiveness of the hybrid material synthesis methodology was confirmed indirectly, using Fourier transform infrared spectroscopy, elemental and colorimetric analysis. Dispersive-morphological analysis indicates that the products with the best properties were obtained using 10 parts by weight of magnesium lignosulfonate per 100 parts of Syloid®244 silica. The relatively high thermal stability recorded for the majority of the synthesized products indicates the potential use of this kind of a material as a polymer filler. Results indicating the high electrokinetic stability of the materials are also of great importance. Additionally, the very good porous structure properties indicate the potential use of silica/lignosulfonate systems as biosorbents of hazardous metal ions and harmful organic compounds.

Immobilization of Amano Lipase A onto Stöber silica surface: process characterization and kinetic studies

Abstract The immobilization of Amano Lipase A from Aspergillus niger by adsorption onto Stöber silica matrix obtained by sol-gel method was studied. The effectiveness of the enzyme immobilization and thus the usefulness of the method was demonstrated by a number of physicochemical analysis techniques including Fourier Transform Infrared Spectroscopy (FT-IR), elemental analysis (EA), thermogravimetric analysis (TG), porous structure of the support and the products after immobilization from the enzyme solution with various concentration at different times. The analysis of the process’ kinetics allowed the determination of the sorption parameters of the support and optimization of the process. The optimum initial concentration of the enzyme solution was found to be 5 mg mL-1, while the optimum time of the immobilization was 120 minutes. These values of the variable parameters of the process were obtained by as ensuring the immobilization of the largest possible amount of the biocatalyst at Graphical Abstract

Functional polypropylene composites filled with ultra-fine magnesium hydroxide

Abstract Magnesium hydroxide was prepared under controlled conditions from aqueous Mg(NO3)2 and NaOH solutions. The small, nanoplate-shaped particle size distribution was monomodal from 164 to 459 nm. Functional polypropylene/Mg(OH)2 and polypropylene/polypropylene 1% maleic anhydride/Mg(OH)2 composites were prepared containing 10% or 30% Mg(OH)2. The composites have a high Young’s modulus (twice that of polypropylene) and comparable tensile strength but less ductility. EDX examination of the fractured composite surfaces suggested a homogeneous Mg(OH)2 distribution for composites produced with the addition of polypropylene grafted with maleic anhydride. The polypropylene/Mg(OH)2 composites showed good antibacterial activity. The polypropylene/polypropylene 1% maleic anhydride/Mg(OH)2 composites were less effective. Graphical Abstract

Synthesis and physicochemical characterization of silicafillers modified with octakis({3-methacryloxypropyl}dimethylsiloxy) octasilsesquioxane

Abstract Hybrid nanofillers of silica grafted with octakis({3-methacryloxypropyl}dimethylsiloxy) octasilsesquioxane were obtained by the method based on solvent evaporation with the use of both hydrated or emulsion spherical silica. Octakis({3-methacryloxypropyl}dimethylsiloxy) octasilsesquioxane was applied as a modifying agent and it was synthesized by employing the hydrosilylation reaction. The effectiveness of modification of the hybrid nanofillers obtained was verified using Fourier transform infrared spectroscopy and nuclear magnetic resonance (29Si and 13C CP MAS NMR). The products obtained were characterized by determination of their physicochemical properties and porous structure, including specific surface area, pore diameter and pore volume. Dispersion degree and particle size of the nanofillers was characterized by NIBS (Non-Invasive Back-scatter) method and laser diffraction technique, while their morphology by transmission electron microscopy.