Zeolite A Synthesis under Dynamic Conditions, after Hydrogel Ageing

Zeolites are crystalline, microporous, alumo-silicate materials (around 400 types) which are used in many applications. Each field of usage (catalysis, ion exchange, sorption, molecular sieving, etc.) has demands regarding crystals’ structural and particulate properties. Detailed understanding of the mechanisms of crystals’ formation and growth enables the control of these properties. Hydrogels of the starting composition 3.2 Na2O × 2 SiO2 × 1.05 Al2O3 × 250 H2O were heated in stainless steel reactor at 80 °C under dynamic conditions, after ageing for tA = 0–209 h at 25 °C. Solid phase samples were characterized using microscopy (OM, SEM), PXRD and laser light scattering (LLS). Specific number of zeolite A crystals was calculated from particle size distributions. It was shown that the some particulate properties: specific number of crystals and crystal size distribution, are changing towards higher number of crystals and wider size distribution while the morphology of the crystals remains the same. Also, the crystal growth rate is higher in the systems which are treated under dynamic conditions. Obtained results were compared with data of systems crystallized under static conditions and commented on the grounds of the autocatalytic nucleation theory. (doi: 10.5562/cca2055

Investigation of Factors Influencing the Precipitation of Iron Oxides from Fe(II) Containing Solutions

Factors that influence the precipitation of iron oxides from Fe(II) containing solutions were investigated by X-ray powder diffraction, 57Fe Mössbauer and FT-IR spectroscopies, FE SEM and EDS techniques. Near spherical aggregates of spindle-shape goethite particles were obtained by oxidation of 0.1 mol dm–3 FeSO4 solution (suspension) with pure oxygen at 90 °C. Wide and thin goethite particles elongated along the crystallographic c-axis were formed in parallel. With the addition of tetramethylammonium hydroxide to 0.1 mol dm–3 FeSO4 solution (suspension) substoichiometric magnetite (Fe3-xO4) particles were additionally formed. They were dominant at pH > 12.5. Mössbauer spectroscopy was used to calculate the stoichiometries of Fe3-xO4 particles. Very small magnetite particles ( 20–100 nm) showed a tendency to aggregate. The twinning effect of octahedral magnetite particles (> 200 nm) was observed. A drastic effect on the properties of iron oxide precipitates was achieved by adding H3PO4 to the precipitation system containing 0.1 mol dm–3 FeSO4 + 0.01 mol dm–3 H2SO4 solution at the start. In dependence on the concentration of the added H3PO4, nanosize goethite particles about 15–25 nm in size, or poor crystalline ferrihydrite particles (two-line ferrihydrite) were obtained. The EDS analyses of the precipitates did not show any significant change in the sulphur content, whereas the phosphorous content gradually increased in the precipitates with an increase in the added H3PO4. In high concentrations phosphates completely suppressed the formation of goethite under given experimental conditions, and phosphated ferrihydrite was formed instead

Kinetic Analysis of Non-isothermal Transformation of Zeolite 4A into Low-carnegieite

Kinetics of the non-isothermal transformation of zeolite 4A to low-carnegieite was investigated by the X-ray diffraction method. Changes in the fractions of zeolite 4A, amorphous aluminosilicate and low-carnegieite during zeolite 4A heating at three different heating rates (0.0833 ° s–1, 0.1667 ° s–1 and 0.333 ° s–1) showed that amorphization of zeolite 4A and crystallization of low-carnegieite take place simultaneously. Kinetic analyses of amorphization and crystallization showed that the non-isothermal transformation took place by the same mechanism as the isothermal transformation, i.e., amorphization of zeolite 4A proceeded by a random, diffusion- limited agglomeration of the short-range ordered aluminosilicate subunits formed by the thermally induced breaking of Si-O-Si and Si-O-Al bonds between different building units of zeolite framework. Crystallization of low-carnegieite occurred by homogeneous nucleation of low-carnegieite inside the matrix of amorphous aluminosilicate and was diffusion-controlled, with one-dimensional growth of the nuclei. Kinetics of non-isothermal processes was determined by the changes of the rate constants during heating and the apparent activation energies of amorphization and crystallization