RESUMO
In order to propose a novel, effective adsorbent of Cu(II) ions, hybrid carbon-mineral nanocomposites with metallic elements (Mn/Fe in the case of B-6, Mn - B-8) were examined. A combination of mechanochemical and pyrolytic methods was used to obtain these bimodal micro-mesopore systems. First, mechanochemical mixing of phenol-formaldehyde resin and inorganic compounds in a ball mill was carried out. Then, the pyrolysis of the mixture under inert atmosphere at 800 °C was performed. The obtained composites were characterized using nitrogen adsorption/desorption, Fourier transform infrared spectroscopy, electron microscopes as well as X-ray diffraction, X-ray fluorescence and X-ray photoelectron spectroscopy. Adsorption, electrokinetic and aggregation studies were also performed, in the absence and presence of poly(acrylic acid) (PAA) - a macromolecular compound commonly used in industry and agriculture, which may be present in wastewater together with copper(II) ions. Under examined conditions (at pH 5 and 6), Cu(II) adsorbed amount was higher on the B-8 surface than on the B-6 one. At pH 6 for the initial Cu(II) concentration 100 ppm, 51.74% of the ions was adsorbed on B-8% and 46.68% - on B-6. Heavy metal adsorption contributes to stronger aggregation of nanocomposite particles. Thus, the presented bimodal solids, especially that containing Mn (called B-8), can be considered as adsorbents in heavy metal removal from aqueous solutions.
RESUMO
The paper presents an original study on adsorption and aggregation phenomena in a mixed system consisting of a macromolecular compound, heavy metal ions and an innovative adsorbent. The authors used ionic polyacrylamides (PAM), Cu(II) ions and carbon-silica composite (C-SiO2) in the experiments. Such a system has not yet been described in the literature and therefore, the article is of significant novelty and great importance. The composite was prepared by mixing phenol-formaldehyde resin with silica and pyrolysis at 800 °C. The adsorbed amounts of Cu(II) ions and PAM were determined spectrophotometrically. C-SiO2 was characterized using potentiometric titration, microelecrophoresis and Fourier Transform Infrared Spectroscopy (FTIR) analysis. In turn, the C-SiO2 aggregation was established turbidimetrically as well as using a particle size analyzer. The obtained results indicated that both Cu(II) ions and ionic polyacrylamide were adsorbed on the composite surface at pH 6. The highest noted adsorbed amounts were 9.8 mg/g for Cu(II) and 35.72 mg/g for CT PAM-25%. Cu(II) ions increased the anionic PAM adsorbed and reduced the cationic PAM one. The adsorption of anionic PAM (50 ppm) stimulated the solid aggregation significantly. What is more, Cu(II) ions enhanced this process. The size of particles/aggregates formed without additives equaled 0.44 µm, whereas in the mixed Cu(II)/AN PAM system, they were even at 1.04 µm.
RESUMO
Metal-carbon nanocomposites possess attractive physical-chemical properties compared to their macroscopic counterparts. They are important and unique nanosystems with applications including in the future development of nanomaterial enabled sensors, polymer fillers for electromagnetic radiation shields, and catalysts for various chemical reactions. However, synthesis of these nanocomposites typically employs toxic solvents and hazardous precursors, leading to environmental and health concerns. Together with the complexity of the synthetic processes involved, it is clear that a new synthesis route is required. Herein, Cu/C, Ni/C and Co/C nanocomposites were synthesized using a two-step method including mechanochemical treatment of polyethylene glycol and acetates of copper, nickel and cobalt, followed by pyrolysis of the mixtures in an argon flow at 700 °C. Morphological and structural analysis of the synthesized nanocomposites show their core-shell nature with average crystallite sizes of 50 (Cu/C), 18 (Co/C) and 20 nm (Ni/C) respectively. The carbon shell originates from disordered sp2 carbon (5.2-17.2 wt.%) with a low graphitization degree. The stability and prolonged resistance of composites to oxidation in air arise from the complete embedding of the metal core into the carbon shell together with the presence of surface oxide layer of metal nanoparticles. This approach demonstrates an environmentally friendly method of mechanochemistry for controllable synthesis of metal-carbon nanocomposites.