Agnieszka Kołodziejczak-Radzimska

Zinc Oxide—From Synthesis to Application: A Review

Zinc oxide can be called a multifunctional material thanks to its unique physical and chemical properties. The first part of this paper presents the most important methods of preparation of ZnO divided into metallurgical and chemical methods. The mechanochemical process, controlled precipitation, sol-gel method, solvothermal and hydrothermal method, method using emulsion and microemulsion enviroment and other methods of obtaining zinc oxide were classified as chemical methods. In the next part of this review, the modification methods of ZnO were characterized. The modification with organic (carboxylic acid, silanes) and inroganic (metal oxides) compounds, and polymer matrices were mainly described. Finally, we present possible applications in various branches of industry: rubber, pharmaceutical, cosmetics, textile, electronic and electrotechnology, photocatalysis were introduced. This review provides useful information for specialist dealings with zinc oxide.

Structural characterisation of ZnO particles obtained by the emulsion precipitation method

Zinc oxide was obtained by precipitation in an emulsion system with zinc acetate used as a precursor of ZnO and potassium hydroxide or sodium hydroxide as a precipitating agent. The cyclohexane, as an organic phase, and a nonionic surfactant mixture were also used for preparation of the emulsion. By applying modifications of the ZnO precipitation process, such as changing the precipitating agent, composition of substrates, and the rate of substrate dosing, some interesting structures of ZnO particles were obtained. The morphology of the modified samples was analysed based on SEM (scanning electron microscope) and TEM (transmission electron microscope) images. Moreover the samples were characterised by determination of their dispersive properties using the noninvasive back scattering method (NIBS), adsorption parameters (BET), and crystalline structure (XRD). Thermogravimetric analysis (TG) as well as infrared spectrophotometry (FT-IR) was also applied. For selected samples their electrical properties (dielectric permittivity and electric conductivity) were also measured. The zinc oxide obtained consisted of particles in the shapes of solids, ellipsoids, rods, and flakes, with size ranging from 164 to 2670nm and showed well-developed surface area with values as high as 20m2/g.

Chitin-Lignin Material as a Novel Matrix for Enzyme Immobilization

Innovative materials were made via the combination of chitin and lignin, and the immobilization of lipase from Aspergillus niger. Analysis by techniques including FTIR, XPS and 13C CP MAS NMR confirmed the effective immobilization of the enzyme on the surface of the composite support. The electrokinetic properties of the resulting systems were also determined. Results obtained from elemental analysis and by the Bradford method enabled the determination of optimum parameters for the immobilization process. Based on the hydrolysis reaction of para-nitrophenyl palmitate, a determination was made of the catalytic activity, thermal and pH stability, and reusability. The systems with immobilized enzymes were found to have a hydrolytic activity of 5.72 mU, and increased thermal and pH stability compared with the native lipase. The products were also shown to retain approximately 80% of their initial catalytic activity, even after 20 reaction cycles. The immobilization process, using a cheap, non-toxic matrix of natural origin, leads to systems with potential applications in wastewater remediation processes and in biosensors.

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

TiO2‐SiO2 inorganic barrier composites: from synthesis to application

Purpose – The purpose of this paper is to report on a method of synthesis of TiO2‐SiO2 oxide composites characterised by spherically shaped particles with sizes in the micrometric ranges, which can be applied as a new generation of textile/TiO2‐SiO2 composites with barrier properties against UV radiation. Synthesis and characterisation of TiO2‐SiO2 oxide composites with a high degree of dispersion were performed, and their influence on the barrier properties of textile fabrics was investigated.Design/methodology/approach – The precipitation was performed with the use of solutions of titanium sulphate and sodium silicate as the precipitating agent, which are cheap alternatives to organic precursors of Ti and Si. The reaction was conducted in an emulsion system, where cyclohexane was used as the organic phase and non‐ionic surfactants NP3 and NP6 as emulsifiers were applied.Findings – The direction of substrate supply, concentration of the reagents and their ratio and other conditions of precipitation proce...

Candida antarctica Lipase B Immobilized onto Chitin Conjugated with POSS® Compounds: Useful Tool for Rapeseed Oil Conversion

A new method is proposed for the production of a novel chitin-polyhedral oligomeric silsesquioxanes (POSS) enzyme support. Analysis by such techniques as X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy confirmed the effective functionalization of the chitin surface. The resulting hybrid carriers were used in the process of immobilization of the lipase type b from Candida antarctica (CALB). Fourier transform infrared spectroscopy (FTIR) confirmed the effective immobilization of the enzyme. The tests of the catalytic activity showed that the resulting support-biocatalyst systems remain hydrolytically active (retention of the hydrolytic activity up to 87% for the chitin + Methacryl POSS® cage mixture (MPOSS) + CALB after 24 h of the immobilization), as well as represents good thermal and operational stability, and retain over 80% of its activity in a wide range of temperatures (30–60 °C) and pH (6–9). Chitin-POSS-lipase systems were used in the transesterification processes of rapeseed oil at various reaction conditions. Produced systems allowed the total conversion of the oil to fatty acid methyl esters (FAME) and glycerol after 24 h of the process at pH 10 and a temperature 40 °C, while the Methacryl POSS® cage mixture (MPOSS) was used as a chitin-modifying agent.

Physicochemical and catalytic properties of acylase I from aspergillus melleus immobilized on amino- and carbonyl-grafted stöber silica

Acylase I from Aspergillus melleus was immobilized on supports consisting of unmodified and modified silica. Modification was performed using 3‐aminopropyltriethoxysilane (APTES) and glutaraldehyde (GA). The effectiveness of immobilization was investigated using the standard Bradford method in addition to a number of physicochemical techniques, including spectroscopic methods (FTIR, 29Si and 13C CP MAS NMR), porous structure and elemental analysis, and zeta potential measurement. A determination of catalytic activity was made based on the deacetylation reaction of N‐acetyl‐l‐methionine. Furthermore, the effect of pH and temperature on the catalytic activity of the free and immobilized enzyme, as well as the reusability of the silica‐bound aminoacylase, were determined. The immobilized systems demonstrated a high degree of catalytic activity. The best catalytic parameters were those of aminoacylase immobilized on silica modified with APTES (apparent activity 3937 U/g, relative activity 61.6%).

An organofunctionalized MgO∙SiO2 hybrid support and its performance in the immobilization of lipase from Candida rugosa

Lipase from Candida rugosa was immobilized on MgO·SiO2 hybrid grafted with amine, thiol, cyano, phenyl, epoxy and carbonyl groups. The products were analyzed using Fourier transform infrared spectroscopy, nuclear magnetic resonance, low-temperature N2 sorption and elemental analysis. Additionally, the degree of coverage of the oxide material surface with different functional groups and the number of surface functional groups were estimated. The Bradford method was used to determine the quantity of immobilized enzyme. The largest quantity of enzyme (25-28 mg/g) was immobilized on the hybrid functionalized with amine and carbonyl groups. On the basis of hydrolysis reaction of p-nitrophenyl palmitate to p-nitrophenol, it was determined how the catalytic activity of the obtained biocatalysts is affected by pH, temperature, storage time, and repeated reaction cycles. The best results for catalytic activity were obtained for the lipase immobilized on MgO∙SiO2 hybrids with amine and carbonyl groups. The biocatalytic system demonstrated activity above 40% in the pH range 4–10 and in the temperature range 30–70 °C. Lipase immobilized on the MgO∙SiO2 systems with amine and epoxy groups retains, respectively, around 80% and 60% of its initial activity after 30 days of storage, and approximately 60–70% after 10 reaction cycles.

Modified and Unmodified Zinc Oxide as Coagent in Elastomer Compounds

Abstract The aim of this work was to study the activity of unmodified and modified ZnO in the peroxide crosslinking of hydrogenated acrylonitrile-butadiene elastomer (HNBR) and ethylene-propylene copolymer (EPM). In the first step, zinc oxide was obtained by emulsion precipitation. Maleic acid was introduced onto the surface of ZnO using an in situ method. The unmodified and modified zinc oxide was characterized using dispersive and morphological analysis, BET surface area analysis, and elemental, spectroscopic and thermal analysis. In the second stage of the research, the ZnO/MA systems were incorporated into the structure of elastomer compounds improving the kinetic and mechanical properties of vulcanizates. The proposed modification method had a favorable effect on the physicochemical properties of the zinc oxide and on the kinetic and mechanical properties of the vulcanizates. This study demonstrated that modification of zinc oxide by maleic acid is a promising technique.